DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States 

Government. Neither the United States Government nor any agency thereof, nor any of 

their employees, nor any of their contractors, subcontractors, or their employees, makes any 

warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, 

completeness, or usefulness of any information, apparatus, product, or process disclosed, or 

represents that its use would not infringe privately owned rights. Reference herein to any 

specific commerical product, process, or service by trade name, trademark, manufacturer, 

or otherwise, does not necessarily constitute or imply its endorsement, recommendation, 

or favoring by the United States Government or any agency, contractor, or subcontractor 

thereof. The views and opinions of authors express herein do not necessarily state or reflect 

those of the United States Government or any agency, contractor, or subcontractor thereof.

Printed in the United States of America

Available from

National Technical Information Service

U.S. Department of Commerce

5285 Port Royal Road

Springfield, VA 22161

BNL-71045

UC400

(General Energy Research)
Activity Report

National Synchrotron Light Source

For the period October 1, 2001 through September 30, 2002

Nancye Wright, Steve Giordano & Lauren Giordano 

May 2003

The National Synchrotron Light Source Department

is supported by the

Office of Basic Energy Sciences

United States Department of Energy

Washington, D.C.

Brookhaven National Laboratory

Brookhaven Science Associates, Inc.

Upton, New York 11973

Under Contract No. DE-AC02-98CH10886

Lisa M. Miller

Patrice Pages

Managing Editor

Science Editor

Design and Layout
ii

Introduction

Introduction by the Chairman

Steve Dierker, Chairman of the National Synchrotron Light Source .......................................................... 1-1

Users’ Executive Committee Report

Leemor Joshua-Tor, Cold Spring Harbor Laboratory, Users’ Executive Committee Chair ........................ 1-2

Science Highlights

Introduction ............................................................................................................................................................................ 2-i

Table of Contents .................................................................................................................................................................. 2-ii

Accelerator Physics............................................................................................................................................................... 2-1

Chemistry ................................................................................................................................................................................ 2-9

Condensed Matter Physics .................................................................................................................................................. 2-23

Geology and Environmental Sciences................................................................................................................................ 2-37

Life Sciences............................................................................................................................................................................ 2-51

Surfaces, Interfaces, and Nanomaterials............................................................................................................................ 2-83

Year in Review

Highlights From the March 2002 American Physical Society Meeting ............................................................................... 3-1

Synchrotron Science Highlighted for Capitol Hill Policymakers................................................................................. 3-3

NSLS’s Podobedov Wins APS Award for Outstanding Thesis Research ... ....................................................................... 3-4

NSLS Annual RapiData Course in X-Ray Crystallography Again Successful............................................................. 3-5

Frontiers in Synchrotron Research on Soft Matter and Biomaterials Workshop ................................................... 3-6

Take our Daughters to Work Day: Mysteries of Light and Extreme Cold Uncovered .......................................... 3-7

Successful Science, Exciting Plans, Record Attendance Characterize This Year’s Annual Users’ Meeting........... 3-8

UEC Community Service Award Presented to Gary Nintzel...................................................................................... 3-12

The Environmental Sciences: Synchrotrons Providing Powerful Tools for a New Science Workshop................ 3-13

X-Ray Sources for Studies of Ultrafast Processes Workshop...................................................................................... 3-14

EXAFS Studies of Nanoscale and Nanostructured Materials Workshop.................................................................. 3-15

Practical Aspects of Membrane Protein Crystallography: From Overexpression to Crystallization Workshop 3-16

Recent Advances in the Application of Synchrotron Radiation to Catalysis Workshop ........................................ 3-18

Combining Synchrotron Infrared and X-Ray Micro-Spectroscopy and Imaging Workshop.................................. 3-19

In situ Studies of Materials Processing Workshop........................................................................................................... 3-20

Advanced Detectors Development Workshop............................................................................................................... 3-22

BNL Hosts VIPs at RHIC, ITD, PET, NSLS....................................... ......................................................................................... 3-23

Secretary Abraham Gives Go-Ahead for BNL Nanoscience Center......................................................................... 3-23

Yongjae Lee Wins Award for High-Pressure Research............................................................................................................. 3-26

NSLS Summer Sunday........................................................................................................................................................... 3-27

BNL Community Summer Science Program: Mount Sinai HS Student Studies at the NSLS................................ 3-27

UEC Lobbying ......................................................................................................................................................................... 3-28

NSLS Annual Awards Ceremony and Picnic..................................................................................................................... 3-29

NSLS Course on EXAFS Data Collection and Analysis ................................................................................................ 3-30

Meeting Report: Low Energy Electrodynamics in Solids (LEES ‘02)............................................................................ 3-31

Learning from Light on “Take Our Sons to Work” Day at the NSLS......................................................................... 3-33
iii

377th Brookhaven Lecture: NSLS’s Elio Vescovo Talks on Thin Magnetic Films....................................................... 3-34

Five BNL Scientists are Granted Tenure ........................................................................................................................... 3-35

NSLS Welcomes U.S. Representative Timothy Bishop................................................................................................... 3-36

NSLS Organization

Organizational Chart............................................................................................................................................................. 4-1

Advisory Committees........................................................................................................................................................... 4-2

Facility Report

Operations, Engineering, and Facility Report

Erik Johnson, Associate Chair for Operations and Engineering................................................................... 5-1

Accelerators Report

James Murphy, Associate Chair for Accelerators........................................................................................... 5-3

User Science Report

Chi-Chang Kao, Associate Chair for User Science ........................................................................................ 5-5

User Administration Report

Mary Anne Corwin, User Administrator......................................................................................................... 5-7

Safety Report

W.R. Casey, Associate Chair for ESH/Q......................................................................................................... 5-9

Building Administration Report

Gerry Van Derlaske, Building Manager..................................................................................... ............................ 5-11

Facility Facts and Figures

Beamline Guide ...................................................................................................................................................................... 6-1

Linac and Booster Parameters............................................................................................................................................ 6-8

VUV Storage Ring Parameters............................................................................................................................................ 6-9

X-Ray Storage Ring Parameters.......................................................................................................................................... 6-10

2002 Ring Performance and Usage .................................................................................................................................... 6-11

Publications

NSLS Users.............................................................................................................................................................................. 7-1

NSLS Staff ................................................................................................................................................................................ 7-28

Abstracts

published on the web at http://nslsweb.nsls.bnl.gov/nsls/pubs/actrpt/2002/Abstracts/

 	


	
 



	
	

	

			

		



 
   

   

 













  !









"  

























 

"
!

" 
 

# $%&#  


$%&







"#
'





$







#

""

(
















)



"




$%& 
* 
   
 
 
 

+
,


-+,.+,

"     
 

  



#


#/



'


"









  0"
 ) 


     
  
" 


/








     +, 
 

 " 















1213

"'

 
  
 
 
 
 
 




0

%



 &$



  '  


!







  " 
 


( 


$21,& 







#






 


 &




-&. 
   4		 

55#





55#





 
 6 7 6


7
-6767.

 55 # "   


89


$21,&

"

'



"

!
"
'

















0		#"

"
!"











0

#"



)
 

 
  

 
 




"






0
#
/










#""
!"$%&








"




 

  

"
 















%#




"

!
"
'
	



 

	



	



	



	







    



 
!

!"
 #

!$%




$&%
	


  ''   
" 

'      #

()*	
%

#

(* 
$

   


$   !

'% 


  #

+

!%!



$



''''$
'#

  

   '
$   %$ 



 


 ,#-#


(

.% 

 


$%!' )



$%


/'
  *$ /0* $
 
 

 
 0
 &
 *$
#


&* %

'
$





1#


'2

12!
'#

' - 

 
  '
$    


$%'
 1'

$$
1- %'
!$

(-

 
'



$
''$

%
#
!'#

'!


$

$

,$
(* %$

#

 

!    


$  % !


%$%%'"

+

$%%$  

'

)+
+
%$+


-$ #



$$


%$

#


$

   
 



!

#


((* 

3

/0*#$

#

 %$
!#

!$   
  0




)!


'$
 


  


4
'!#




$



 %+''



''
+

#


      

  
$ 



$

,
'$ (* 
#


%$
'%%$




!	'#


 
$$'$


$   '
%
+   

$!$ 



%
+!4 

 %$''


'
	'
'$


+$'

'!

.% 5  %'


 '! 3  %     

	'
!
$#


$'


$ (*!6


1 %  !   
 


%$ (*$-*

2(($7

2 - Introduction

Science at the NSLS

Patrice Pages

Science Writer, NSLS

The following pages contain a representation of the outstanding science 

published by NSLS users in 2002. 

Due to space limitations, we have 

chosen to highlight only a portion of 

the scientific accomplishments from 

last year, but we think that these 

articles illustrate the quality and 

breadth of NSLS research. 

The following stories contain a wealth 

of information in a wide range of 

scientific fields and provide an update on important scientific topics. 

For example, you will discover how 

bacteria resist antibiotics (page 2-71) 

or how a certain type of protein is 

involved in cancer (page 2-62). You 

will read about new ways to immobilize contaminants 

in soil (page 2-47), and you will learn how scientists 

have created “light tweezers” to study the electronic 

properties of solids (page 2-28).

The stories are organized into two 

categories: “feature” stories, which 

are geared not only to the NSLS 

user community but also to a more 

general audience, and “highlights”, 

which are more specifically aimed 

at the scientific community. I have 

particularly enjoyed working with 

the NSLS users on these stories, 

and I would like to thank the scientists whom I interviewed to write 

the feature stories and those who 

authored the highlight stories and 

patiently allowed me to edit them. 

I hope that you will share with me 

the excitement generated by the following stories, 

and I will be delighted to hear your impressions about 

them. 
NSLS Activity Report 2002 2 - 

Accelerator Physics

Blue Light Special at the DUV-FEL ........................ ................................ 

2-1

Deep Ultraviolet Free Electron Laser Reaches New Milestone using BNL’s Unique 

HGHG Process ........................................................................................................ 2-3

Very Intense, Terahertz Light Created for the First Time ................................................ 2-5

Nonlinear Harmonic Radiation from a Visible Self-Amplified Spontaneous Emission 

Free Electron Laser

A. Tremaine, A. Murokh, C. Pellegrini, S. Reiche, J. Rosenzweig, M. Babzien, I. Ben-Zvi, R. Malone, 

G. Rakowsky, J. Skaritka, X. Wang, V. Yakamenko, R. Carr, M. Cornacchia, H.-D. Nuhn, R. Ruland, 

L. Bertolini, M. Libkind, A. Toor, and K. Van Bibber ........................................................ 2-7

Chemistry

At the NSLS, NIST, Dow Scientists Reveal Catalysts’ Private Lives ............. ..................... 2-9 

Curbing Nitric Oxide in Car Exhaust............................................................................ 2-10

Discovery of a New Molecular Sieve: Zeolite SSZ-55

M.G. Wu, M.W. Deem, S.A. Elomari, R.C. Medrud, S.I. Zones, T. Maesen, C. Kibby, 

C. Y. Chen, and I. Y. Chan .....................................................................................

2-13

Role of Oxygen Vacancies in the Reduction of Nickel Oxide by Hydrogen

J.A. Rodriguez, J.C. Hanson, J.Y. Kim, and A.I. Frenkel ................................................... 2-15

Investigation of the Role of Nickel in the Regulation of the Cell Cycle

F. Al-Mjeni, T. Ju, T.C. Pochapsky, and M.J. Maroney ........................................................ 2-17

Synthesis and Characterization of Carboxylate-FeOOH Nanoparticles (Ferroxanes) and 

Ferroxane-Derived Ceramics

J. Rose, M.M. Cortalezzi, A.R. Barron, M.R. Wiesner, A. Masion, S. Moustier, J.-Y. Bottero 

and P. Bertsch .................................................................................................... 2-19

A Catalyst in Action: Structure and Bonding of Supported Iridium Nanoclusters During 

Propene Hydrogenation Catalysis Determined by EXAFS and Infrared Spectroscopies

A.M. Argo, J.F. Odzak, and B.C. Gates ......................................................................... 2-21

Condensed Matter Physics

Origin of Superconductivity in Fullerenes Still a Mystery ................................................ 2-23

Conducting-Insulating Materials Reveal Their Secrets.................................................... 2-25

BNL, NIST, Norway Gain New Insight into the Superconductivity of MgB2 ...................... 2-26

Scientists Create ‘Light Tweezers’ to Study the Electronic Properties of Solids................... 2-28

Quasiparticles Refuse to Go Away in High-Temperature Superconductors

Science Highlights
2 - Introduction

Condensed Matter Physics (cont.)

Probing Local Magnetic Order in Transition Metal Oxides

Q. Qian, T.A. Tyson, C.-C. Kao, M. Croft, and A. Yu. Ignatov ............................................ 2-33

Imaging Single Dopant Atoms and Clusters in Bulk Silicon

P. Voyles, D. Muller, J. Grazul, P. Citrin, and H. Gossmann ............................................... 2-35

Geology and Environmental Sciences

Scientists Provide Evidence that Life May Have Come From Comets ................................ 2-37

SBU Researchers at the NSLS Discover Properties of Perovskite, Explain 

Why No Earthquakes Start in Earth’s Lower Mantle ....................................................... 2-40

Osmium is Stiffer Than Diamond

H. Cynn, J.E. Klepeis, C.-S. Yoo, and D.A. Young .......................................................... 2-43

Modeling Sulfur K-XANES Spectra of Humic Acids With the Principal Component 

Analysis Approach

S. Beauchemin, D. Hesterberg, and M. Beauchemin ....................................................... 2-45

Influence of Aging and pH on Dissolution Kinetics and Stability of Pyromorphite

K.G. Scheckel and J.A. Ryan .................................................................................... 2-47

Slow Precipitation and Dissolution of Solids Affects the Mobility of Heavy Metals in Soils

A. Voegelin, A.C. Scheinost, K. Bühlmann, K. Barmettler, and R. Kretzschmar ....................... 2-49

Life Sciences

Enzyme Studies May Lead to New Antiviral Agents........................................................ 2-51

Anti-Alzheimer’s Drug Mechanism Revealed with X-Rays................................................ 2-53

Scientists at NSLS Discover How Papillomavirus ‘Unzips’ DNA......................................... 2-55

Biological Serendipity: Molecular Details of Cell Membrane Fusion Revealed ..................... 2-58

Role of Cancer Protein Identified by Princeton, LBNL Team at NSLS................................. 2-60

Scientists Uncover Molecular Clues about Origin of Cancer ............................................. 2-62

Kinetics of Association Between the Integration Host Factor and DNA in Escherichia coli

G.M. Dhavan, M. Brenowitz, M.R. Chance, and D.M. Crothers ............................................ 2-65

Structural Basis of Gating by the Outer Membrane Transporter FecA

A.D. Ferguson, B.S. Smith, J. Deisenhofer, R. Chakraborty, L. Esser, and D. van der Helm ........

2-67

Structural Identification of a Bacterial Quorum Sensing Signal Containing Boron

X. Chen, S. Schauder, I. Pelczer, L. Bassler, F. M. Hughson, N. Potier, and A. Van Dorsselaer ...... 2-69

Scientists Show that Resistance to Aminoglycoside Antibiotics is Due in Part to 

Target Mimicry

D.H. Fong and A.M. Berghuis .................................................................................. 2-71
NSLS Activity Report 2002 2 - 

A Novel Mechanism for Clostridium Botulinum Neurotoxin Inhibition

S. Eswaramoorthy, D. Kumaran, and S. Swaminathan .....................................................

2-73

Identification of the 22nd Genetically-Encoded Amino Acid in a Methanogen Methyltransferase

G. Srinivasan, T.K. Ferguson, C.M. James, B. Hao, W. Gong, J. Krzycki, and M. Chan ............... 2-75

Structure of Human Nicotinamide/Nicotinic Acid Mononucleotide Adenylyltransferase (NMNAT)

T. Zhou, D.R. Tomchick, D.D. Binns, N.V. Grishin, H. Zhang, O.V. Kurnasov, A.L. Osterman, and 

V.E. Marquez ....................................................................................................... 2-77

Structure of a Bacterial ATP-Binding Cassette Transporter

K.P. Locher, A.T. Lee, and D.C. Rees .... ................................................................

2-79

X-ray Structure of the Rotavirus Protein Involved in Genome Replication and Packaging

H. Jayaram, Z. Taraporewala, J.T. Patton, and B.V. Venkataram Prasad ................................ 2-81

Surfaces, Interfaces, and Nanomaterials

At the NSLS, BNL Scientists Create Stripes, Islands, Towers........................................... 2-83

Scientists Create New Material with Varying Densities of Gold Nanoparticles..................... 

2-85

Nanoscale Crystallography Reveals Structural Details.................................................... 2-87

New Technique Reveals Structure of Films with High Resolution...................................... 2-88

Molecular Film on Liquid Mercury Reveals New Properties .............................................. 2-90

Tailor-Made Polymer Nanocrystals

L. Zhu, P. Huang, W.Y. Chen, Q. Ge, R.P. Quirk, S.Z.D. Cheng, E.L. Thomas, B. Lotz, B.S. Hsiao, 

F. Yeh, and L. Liu .................................................................................................. 2-93

Nanoscale Self-Assembly of Thin-Film Molecular Materials for Electro-Optic Switching

M.E. van der Boom, P. Zhu, G. Evmenenko, J.E. Malinsky, W. Lin, P. Dutta, and T.J. Marks .........

2-95

Structures of Quantum Wires in Gold/Silcon(557)

I. Robinson, P. Bennett, and F. Himpsel ....................................................................... 2-97

Formation of Alkylsilane-Based Monolayers on Gold

T.M. Owens, K.T. Nicholson, M.M. Banaszak Holl, and S. Süzer .......................................... 

2-99
Accelerator

Physics
2 - 1 Accelerator Physics

Blue Light Special at the DUV-FEL

February 13, 2002 - A specially

intense blue light shone for the first

time at BNLís Deep Ultra-Violet Free

Electron Laser (DUV-FEL). On hand

to see this 400-nanometer (billionths of a meter) wavelength light

were NSLS scientists Adnan

Doyuran, Bill Graves, Henrik Loos,

Timur Shaftan, Brian Sheehy, and

Li-Hua Yu, with technical specialist

Phil Marino. It was a satisfying and

visible reward for the hard work

of many.

ìAchieving this 400-nanometerwavelength light is an important

milestone in the development of

the DUV-FEL,î says Erik Johnson,

the NSLSís DUV-FEL Project Manager. ìIt paves the way to producing even shorter and more intense

100-nanometer-wavelength laser

light.î

Visible lightís wavelength ranges

from 400 to 700 nanometers (nm).

When it produces the more energetic 100 nm light, the DUV-FEL

will become an important tool for

studying chemical reactions.

The commissioning experiment, led

by Yu, achieved the visible 400-nm

light by Self Amplified Spontaneous Emission (SASE).

The experiment demonstrated that

the components of the machine

work successfully and have been

appropriately tuned. The scientists

also found that the light intensity

was about 600 times higher than

anticipated.

ìWe were pleasantly surprised by

how intense the output light was,î

says Johnson. At least two factors

contributed to this high output and

its comparatively rapid attainment,

he explains: The high quality of the

beam generated by the linear accelerator, and the beam alignment,

which allows rapid and precise correction of the beam trajectory.

ìHowever, light produced by the

SASE process is just the starting

point for the DUV-FEL program,î

Johnson says.

The project has its roots in earlier

work. In 1999, in what was an important milestone for the field, the

High Gain Harmonic Generation

(HGHG) process in an FEL was

tested for the first time by a team

of scientists led by Yu.

This experiment at BNLís Accelerator Test Facility used a 10 micrometer-wavelength infrared laser to

provide a coherent starting signal

for the lasing process. Some of the

same scientists involved in the successful HGHG experiment are now

planning to extend that work to

wavelengths down to 100 nanometers or fewer at the DUV-FEL.

BNLís DUV-FEL will complement the

NSLS in many ways. The DUV-FELís

pulses of light are up to 1,000 times

shorter than those produced at the

NSLS, enabling the study of time

dynamics of molecules and chemical reactions. DUV-FEL light is also

coherent, meaning that the particles of light, or photons, move like

soldiers following marching orders,

in contrast to incoherent light, in

which the photons follow their own

pace.

The FELís coherent light will have a

peak intensity more than a billion

times higher than that of the NSLS.

ìThe high power and short

timescale of FEL light is expected

to open entirely new fields of research in much the same way that

the NSLS rings did 20 years ago,î

says NSLS physicist William

Graves, who led the electron beam

development effort at the DUV-FEL.

ìThe NSLS will continue to be invaluable to a broad user community, while the FEL will provide enWhile many people were involved in the development and installation of the DUVFEL machine, a smaller core of individuals carried out the commissioning and

initial SASE experiment. Among them: (from left) Richard Heese, Jim Rose, Phil

Marino, Timur Shaftan, Li-Hua Yu, (seated) Boyzie Singh, William Graves, Adnan

Doyuran, Henrik Loos, and Brian Sheehy. (Not in photo, Joe Greco, Erik Johnson.)
Feature Articles 2 - 2

hanced capabilities for some specialized experiments.î

The DUV-FEL is one of just a handful of FELís in the world designed

to operate in the ultraviolet, and it

is the only facility designed to generate light through the HGHG process.

ìIt is also an important resource

for the FEL research community

right now,î Graves says, ìbecause

most of the other similar FEL programs are shut down for upgrades

or are under construction. For a

period of about a year, we are the

only game in town for doing this

kind of work, which will increase

our collaboration with scientists

from DESY [German Synchrotron

Laboratory] and SLAC [Stanford

Linear Accelerator Center].î

According to Johnson, the prospects for the facility are bright.

ìProduction of light at wavelengths

below 400 nm is planned in the

coming year, experimental use of

the laser for chemical physics experiments should begin, and it will

continue to provide a platform for

exploring upgrade paths for the

NSLS scientific program.

 -Patrice Pages

BNLís Deep Ultra-Violet Free Electron

Laser uses fast-moving electrons traveling at close to the speed of light.

They are produced in a photo-injector and brought to their high energy

by a linear accelerator. They then pass

through an undulating magnetic field

in a ìwigglerî device that forces them

to wiggle, and thus to emit light.

SASE

In the Self Amplified Spontaneous

Emission (SASE) process, the FELís

output light gets its start from ìnoise,î

or random signals, that naturally happen in the wiggler.

HGHG

In the High Gain Harmonic Generation (HGHG) process, the FELís output light starts from the fast-moving

electrons interacting with a laser

called the ìseedingî laser. The conditions are set so that the output light

has a frequency that is a harmonic,

or a multiple, of the frequency of the

input laser light.

Similarly to the way one can strike a

key on a piano and set the strings of

higher octaves in motion, the HGHG

process shifts the wavelength of the

seeding laser to a higher frequency,

generating a wavelength for the output light, the HGHG light, that is beyond the range of the original laser.

In addition, the coherence, or orderliness, of the seeding laser is imparted

to the output DUV-FEL light, providing a light beam that is significantly

more coherent than light produced

from SASE sources.

Learn About the SASE and HGHG Processes

Many of the National Synchrotron Light

Sourceís Deep Ultra-Violet Free Electron

Laser team are gathered in the Source

Development Laboratory, celebrating

the successful effort to achieve a 400-

nanometer wavelength beam of light.

[Editorís note: Reprinted with permission from the BNL Bulletin - April 12,

2002.]
2 - 3 Accelerator Physics

November 1, 2002 - After three

years of intense effort in developing a new source of laser light called

a deep ultra-violet free electron laser (DUV-FEL), BNL scientists generated very intense ultraviolet light

by a process called high gain harmonic generation (HGHG). This

process, unique to BNL, was developed under the direction of LiHua Yu, a physicist at the NSLS.

HGHG will ultimately generate deep

ultraviolet laser light with unsurpassed brightness.

ìSuch intense light,î Yu says,î will

be a powerful new tool that will

reveal fine details of atomic interactions inside materials and the

very fast motions of molecules in

chemical reactions all this with a

precision unequaled so far.î

By using the HGHG process, the

DUV-FEL seeks to achieve very

short wavelengths of light. While

visible lightís wavelengths range

from 400 nanometers (nm) for blue

light to 700 nm for red light - a

nanometer being a billionth of a

meter - the wavelength of the light

produced at the DUV-FEL last week

was 266 nm. The HGHG process

also generated significant deep ultraviolet light at 88 nm.

The advantages of two current light

sources will be combined in the

DUV-FEL. By generating very intense deep ultraviolet light, the

DUV-FEL will act like a synchrotron,

which delivers short wavelengths

but less intense light, and a laser,

which produces very intense light,

but only at longer wavelengths.

Over the last three years, the DUVFEL has been advancing through

many steps, each step representing a new technological challenge.

The many NSLS scientists, engiDeep Ultraviolet Free Electron Laser Reaches New Milestone

Using BNLís Unique HGHG Process

neers, and technicians who made

key contributions to overcome

these challenges include physicists

William Graves, Erik Johnson,

Samuel Krinsky, Timur Shaftan,

and Brian Sheehy; postdoctoral

research associates Adnan Doyuran

and Henrik Loos, mechanical engineer John Skaritka, and radio frequency engineer Jim Rose. The

experiment also benefited greatly

from the scientific contributions of

Ilan Ben-Zvi, Richard Heese,

George Rakowsky, Xijie Wang, and

Zilu Wu; the computer control of

Kate Berman; and the technical

assistance of Joseph Greco, Dave

Harder, Michael Lehecka, Phil

Marino and Boyzie Singh.

ìIn addition,î says Yu, ìvaluable

contributions were made by other

scientists in past stages of the DUVFEL. The team spirit of all who have

worked on the project helped in

achieving the present milestone.î

Yu explains that the DUV-FEL can

produce such intense light because

of a property called ìcoherence.î

In both a synchrotron and an FEL,

electrons are accelerated to near

the speed of light, and then are

forced to emit very intense light by

going through magnets that bend

their trajectories. But while light is

emitted at random, or ìincoherently,î in a synchrotron, it is produced ìcoherently,î in the DUV-FEL,

leading to a dramatic increase in

intensity, which can be up to 10

million times as intense as current

synchrotron light.

ìIt is as if, instead of having a group

of people singing the same song at

different times, they sang in unison,î says Shaftan.

Interim Lab Director Peter Paul (right) celebrates the latest milestone at BNLís

DUV-FEL with National Synchrotron Light Source (NSLS) Department members

(foreground, from left) Li Hua Yu, James Murphy, Adnan Doyuran, NSLS Chair

Steve Dierker; (back, from left) Timur Shaftan, John Skaritka, Boyzie Singh, Erik

Johnson, Henrik Loos, and Brian Sheehy.
Feature Articles 2 - 4

In the DUV-FEL, the electrons can

ìsing in unisonî in two different

ways, called self-amplified spontaneous emission (SASE) and HGHG.

In the first process, electrons interact with light emitted by their

fellow electrons, creating small

groups of electrons. ìInside each

group, all the electrons sing in unison, but the songs between two

groups are out of sync,î Shaftan

says.

In the HGHG process, the electrons

interact with light provided by a

laser at the entrance of the DUVFEL, a process leading to groups of

electrons, as before, but ìthis time,

not only do you have a united choir

in each group, but all groups sing

together,î Loos says. ìThis ësuperchoirí of electrons generates light

that is many times more intense

than the one generated by the

SASE process.î

While many FELs are currently under development throughout the

world, they are all based on the

SASE process. Brookhavenís DUVFEL is the only FEL using the HGHG

process, which will allow it to generate the brightest deep ultraviolet light so far. Unlike SASE, HGHG

also generates light at wavelengths

that are fractions (one-half, onethird, one-quarter, etc.) of the input wavelength.

 ìSuch harmonics can be generated

by conventional lasers when they

cross a given crystal or gas,î

Doyuran says. ìBut the intensity of

these harmonics is much weaker

than the input light. The big advantage of HGHG is that the harmonics are much more intense

than those produced with a conventional laser.î

To benefit from this very intense

light, three BNL scientists from the

Chemistry Department have already submitted proposals to use

the DUV-FEL.

Arthur Suits is interested in using

light-induced dissociation of atoms

in hydrocarbons to reveal details

of their molecular structure and

bonding. ìThe DUV-FEL is really

ideal for our experiments,î he says.

ìThe information we hope to gain

using it would be impossible to

obtain by other means.î

Louis DiMauro plans to use the

DUV-FELís short and highly intense

light pulses to study the interaction of matter with intense, shortwavelength light. ìThis tool will

open up many new areas of research in fundamental and applied

science,î he says.

Michael White intends to use the

DUV-FEL to study chemical reactions that occur on the surfaces of

materials, for which the product

yields are low or where the gaseous products are particularly difficult to detect.

Says White, ìIn the long term, the

DUV-FEL will produce very short

pulses that will provide new information on surface processes in real

time.î

For Yu and his collaborators, these

proposals are a clear sign that the

efforts of the past three years are

coming to fruition.

ìThe scientific use of the DUV-FEL

will be the best reward for all of us

and the crowning of a lot of hard

work and dedication from the scientists, engineers and technicians

who worked on this project,î says

James Murphy, NSLS Associate

Chairman for Accelerators.

The National Synchrotron Light

Source Department team working

on BNLís deep ultraviolet free

electron laser include: (front, from

left) Timur Shaftan, Richard

Heese, Boyzie Singh, Adnan

Doyuran, Phil Marino, and Li Hua

Yu; (middle, from left) Joe Greco,

James Murphy, Xijie Wang, Bill

Bambina, Sorin Pop, Brian

Sheehy, Zilu Wu, and James Rose;

(back, from left) Henrik Loos, Erik

Johnson, and John Skaritka.

 -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - November

8, 2002.]
2 - 5 Accelerator Physics

Scientists report in the November

14, 2002 issue of Nature that they

have created a beam of radiation

that has never been produced before. The beam, which contains a

broad spectrum of frequencies up

to about one terahertz - or a trillion of cycles per second - and a

brightness 20,000 times higher

than that of previous terahertz

beams, was produced at the U.S.

Department of Energyís Thomas

Jefferson National Accelerator Facility in Newport News, Virginia.

ìOne of the anticipated applications

for this terahertz radiation is imaging,î says Larry Carr, a physicist

at the NSLS, and lead author of the

study. ìTerahertz radiation can penetrate many centimeters inside

materials, allowing one to ëseeí

whatís inside.î

Other potential applications of the

newly created terahertz radiation

Very Intense, Terahertz Light Created for the First Time

include better detection of concealed weapons, hidden explosives

and land mines; ìfingerprintingî of

chemical and biological terror materials in envelopes, packages or

air; and widening the frequency

bands available for wireless communication.

The powerful terahertz radiation

was produced in an experiment

conceived and led by Gwyn Williams, physicist at Jefferson Lab. He

and his collaborators, from

Brookhaven and Lawrence Berkeley National Laboratories, sent a

beam of electrons at nearly the

speed of light inside an accelerator, in which they were deflected

by a magnetic field, causing them

to emit radiation. Inside the accelerator, the electrons were squeezed

into small bunches (less than 1

millimeter long), inside which they

emitted radiation in unison.

ìProducing intense light pulses by

this method dates back to more

than 10 years ago,î Carr says, ìbut

the pulse rate was limited to just a

few times each second. Now, we

can accelerate 75 million electron

bunches each second, which creates a stream of terahertz pulses

delivering the unprecedented average power of 20 watts.î

As with any new technology, the

most important applications of

terahertz radiation are not known

so far, but the authors of the study

are confident that it can potentially

extend and add to the wave-based

technologies that have defined the

last century and a half. ìThe growing awareness of the usefulness of

terahertz radiation is like what happened a century ago with X-rays -

only terahertz radiation will have a

much wider range of applications,î

Williams says.

NSLS Physicist Larry Carr (left) and Jefferson Lab Physicist Gwyn Williams working on the experiment that recently produced

very powerful terahertz radiation.

-Patrice Pages
2 - 7 Accelerator Physics

FUNDING

U.S. Department of Energy (DOE)

PUBLICATION

A. Tremaine et al. ìExperimental Characterization of Nonlinear Harmonic

Radiation from a Visible SASE FEL at

Saturationî, Phys. Rev. Lett., 88, 204801

(2002).

FOR MORE INFORMATION

Aaron Tremaine, Department of

Physics and Astronomy, University of

California, Los Angeles

tremaine@stout.physics.ucla.edu

BEAMLINE

ATF3

Nonlinear Harmonic Radiation from a Visible

Scientists from the University of California, Los Angeles, Brookhaven

National Laboratory, Stanford Linear Accelerator Center and Lawrence

Livermore National Laboratory have demonstrated for the first time the

feasibility of using nonlinear harmonic self-amplified spontaneous emission (SASE) free electron laser (FEL) radiation to produce coherent,

femtosecond x-rays. Nonlinear harmonic radiation (NHR) was observed

using the visible-to-infrared SASE amplifier (VISA) FEL at saturation.

Self-Amplified Spontaneous Emission Free

Electron Laser

A. Tremaine1, A. Murokh1, C. Pellegrini1, S. Reiche1, J. Rosenzweig1, M. Babzien2,

I. Ben-Zvi2, R. Malone2, G. Rakowsky2, J. Skaritka2, X. Wang2, V. Yakamenko2,

R. Carr3, M. Cornacchia3, H.-D. Nuhn3, R. Ruland3, L. Bertolini4, M. Libkind4,

A. Toor4, and K. Van Bibber4

1

University of California, Los Angeles; 2Brookhaven National Laboratory; 3Stanford Linear

Accelerator Center; 4Lawrence Livermore National Laboratory

The growth of synchrotron light

source applications in the last few

decades is due largely to the improved brightness of the x-ray

beams they produce. During this

same period, high power,

femtosecond-laser technologies

have opened new frontiers in spectroscopy and dynamics system

studies. The free electron laser

(FEL), which produces coherent,

femtosecond x-rays, can bridge

these technologies. Due to the lack

of x-ray seeds and mirrors, all proposed x-ray FELs are based on selfamplified spontaneous emission

(SASE), which is a high-gain,

single-pass FEL amplifier.

We report here the results from a

light source called visible-to-infrared SASE amplifier (VISA) FEL,

which served as research and development for the linear accelerator (linac) coherent light source

(LCLS), a 1-angstrom (Å) FEL to

be built at the Stanford Linear Accelerator Center (SLAC) in California. VISA exemplifies that future

facilities can use SASE nonlinear

harmonic radiation (NHR) to produce narrower bandwidth and

harder x-rays compared to the fundamental radiation.

A major challenge for the VISA collaboration was to implement the

technologies necessary to reduce

the size and cost of FELs, which

could be considerable for future

devices. Using the high-brightness

beam generated by beamline 3 of

Brookhaven National Laboratoryís

Accelerator Test Facility, and a

novel magnetic undulator built by

SLAC, VISA demonstrated the

shortest visible gain length to date

with fundamental saturation after

a distance of only 3.8 meters.

NHR accompanies the fundamental radiation only in the SASE high

gain regime. Figure 1 shows the

superimposed VISA spectrum at

the end of the undulator for the

three lowest FEL modes. The fundamental spectrum is centered at

845 nanometers (nm), and, as expected, the second and third nonlinear harmonics are centered at

422 and 280 nm, respectively.

Gain lengths for each mode are

calculated from the data shown in

the log-linear plot of Figure 2. A

fundamental gain length of Lg

=19 centimeters (cm) is measured,

and NHR gain lengths of 9.8 cm and

6 cm are obtained for the second

and third NHR, respectively, using

only the data in the nonlinear regime. The NHR grows faster than

the fundamental by Lg,n = Lg,1 /

n, verifying theoretical predictions.

By the undulator exit, the energies

of the second and third NHRs are

two percent and one percent of the

fundamental energy, respectively,

confirming theoretical predictions.

Our results show that high-gain

SASE FELs generate substantial

power and narrow spectra for the

Aaron Tremaine
Science Highlights 2 - 8

Figure 2. Measured Energy vs. distance for the

fundamental, second and third nonlinear

harmonics along the second half of the 4-meter

undulator. The gain lengths are 19, 9.8, and 6.0

cm respectively. The energies at the undulator

exit are 52, 0.93, and 0.40 microjoules,

respectively.

Figure 1. SASE FEL spectra

at saturation, showing

fundamental, second and

third harmonics. The

fundamental is highly

attenuated to be on the same

scale as the other modes.

The resolution of the

spectrometer is about 1 nm.

NHR. We measured about five

megawatts of 280-nm (third harmonic) NHR, an impressive power

considering our relatively small system. Extending these results, the

third NHR for the LCLS will be

peaked narrowly around 0.33 Å

with power several orders of magnitude larger than current thirdgeneration synchrotron light

sources.

Magnetic undulator which helped to demonstrate

that coherent, femtosecond x-rays can be

produced by using nonlinear harmonic SASE-FEL

radiation.

Wavelength (nm)

Amplitude

(Count Number)

Energy (nJ)

z(m)

Harmonic Energy vs. Distance
Chemistry
2 - 9 Chemistry

What do car interiors, adhesives,

and sterilizing agents have in common? They are all produced from

propylene oxide, a volatile, colorless liquid with a $10 billion-annual

market value.

At the NSLS, scientists who work

for the National Institute of Standards & Technology (NIST) in

Gaithersburg, Maryland, and Dow

Chemical in Midland, Michigan, are

studying how to produce propylene

oxide in a single-step, environmentally friendly way.

To help in their investigations, they have designed

and built a state-of-the-art

instrument that is now

producing very exciting results.

Propylene oxide is produced by combining propylene, a flammable gas

obtained by breaking up

petroleum molecules, with

oxygen. The process is

accelerated by chemicals

which act as catalysts.

ìSelecting the best catalysts is usually done by

testing different chemicals

and choosing the one with

the best results,î says

Daniel Fischer, NIST physicist and team leader. ìInstead, we are developing

a new method that reveals

the complex transformations that occur during a

chemical reaction. With

that knowledge, we may

be able to develop cleaner and

more efficient catalysts for propylene oxidation.î

To study the role of two types of

catalysts, platinum on alumina and

At the National Synchrotron Light Source at Brookhaven

NIST, Dow Scientists Reveal Catalystsí Private Lives

zeolites, which are cage-like molecules, Fischer and his colleagues

use a technique called near-edge

x-ray absorption fine structure

(NEXAFS).

In NEXAFS, very intense x-rays are

projected toward a cell containing

the reactants and the catalyst. By

precisely tuning the wavelength or

ìcolorî of the x-rays, the scientists

select x-rays with low-energy, soft

x-rays, which probe every step of

the chemical reaction.

The soft x-rays are scattered or reemitted by the chemicals, then

analyzed by a detector. The detector produces a spectrum of signals,

each providing information on the

chemical bonds between the atoms

present in the reactants and the

catalyst.

ìThe signals act like fingerprints,î

says Fischer. ìYou can watch bonds

form and break as the signals wax

and wane with time. It is like looking inside a black box, the eyes

being the detector and the synchrotron radiation providing the illumination.î

Getting clearly separated signals,

however, was not easy. When the

scientists first looked at their

NEXAFS spectra six years

ago, the signals of interest

were camouflaged by many

others.

So Fischer and NIST

postdoc Sharadha

Sambasivan developed and

refined an instrument that

would filter the x-rays coming off the reaction cell by

reflecting the desirable xrays and absorbing the others. The instrument, called

a normal incidence focusing

multi-layer mirror, is a

state-of-the-art device that

dramatically reduces the

background.

ìThe originality of this work

is in being able to understand how these reactants

and catalysts work together

under real conditions,î

Fischer says. ìNow we have

the tools to really find out

what is going on at the

atomic level in catalysts at

work to catch a glimpse of

their private lives!î

 -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - February

8, 2002.]

At the National Synchrotron Light Source, National

Institute of Standards & Technologyís Dan Fischer (front)

and former Dow Chemical chemist Simon Bare prepare

equipment for a catalysis experiment.
Feature Articles 2 - 10

Smog and acid rain could be reduced in large cities if nitric oxide

could be removed from car exhaust.

Nitric oxide, which also causes skin

irritation and blood damage, is usually destroyed inside a carís catalytic converter, but existing catalysts are unable to meet new standards for pollution control and fuel

efficiency.

Now, funded by DOEís Division of

Chemical Sciences, Geosciences &

Biosciences in the Office of Basic

Energy Sciences, Oak Ridge National Laboratory (ORNL) scientists

working at the NSLS have unveiled

some of the inner workings of a

compound that promises to curb

carsí nitric oxide emissions more

efficiently.

For the last four years, led by ORNL

Curbing Nitric Oxide In Car Exhaust

chemist Dave Mullins, the scientists

have been looking at how a catalyst - a material used to accelerate

chemical reactions - made of cerium oxide and rhodium, could be

improved to destroy nitric oxide in

car catalytic converters.

ìIn a carís catalytic converter, nitric oxide is broken down into nitrogen gas and oxygen,î Mullins

says. ìUntil now, catalysts have

been selected hit or miss, so very

little is known about how they actually work.î

The scientists use model catalysts

either powders made of cerium

oxide and very finely dispersed

particles of rhodium or thin oxide

films grown in vacuum and pass

reactant gases over them. Then

they direct x-rays produced by the

NSLS toward the samples while

adjusting the sample temperature

or reactant gas composition. Acting as a camera, the x-rays produced ìsnapshotsî of how the catalyst broke the nitric oxide gas apart.

Two processes, called photoemission and photoabsorption, allowed

the scientists to get a glimpse at

the nitric oxide breakup mechanism.

In the photoemission process, light

absorbed by the compounds ejects

tiny particles called electrons. By

measuring the energies of these

electrons, the scientists can determine the identities of gases

adsorbed on the catalyst. In the

photoabsorption process, light that

is absorbed by the catalyst provides

complementary information about

the composition of the catalyst itself. These experiments confirm

that the rhodium particles are the

movers and shakers responsible for

destroying nitric oxide.

ìThe rhodium particles first weaken

the bond between nitrogen and

oxygen,î Mullins explains. ìThen

the nitrogen is released as a gas,

and the oxygen goes into the cerium oxide or reacts with surrounding hydrogen and carbon, leading

to water and carbon dioxide, respectively.î

Much to their surprise, the scientists also found that the rhodium

particles were being influenced by

the cerium oxide.

ìWe thought that a rhodium particle and the cerium oxide were as

independent as an object sitting on

a table,î Mullins says, ìbut you can

get indirect interactions between

the powder and the particles.î

The interaction between the

rhodium and the cerium oxide

Dave Mullins makes the rhodium more active,
2 - 11 Chemistry

increasing its ability to break the

nitrogen-oxygen bond, Mullins

adds.

Adding impurities in the cerium

oxide can also make it work better,

the scientists observed. After trying various types of impurities, they

noticed that zirconium, a steel-gray

metal used in alloys and ceramics,

ìdramatically improved the ability

of the cerium oxide to exchange

oxygen,î Mullins says.

The scientists also looked for ways

to reduce the temperature at which

nitric oxide is broken down. Much

of the pollution emitted by an automobile is produced just after a

car is started, before the engine

and catalyst reach their operating

temperature. Reducing the temperature for nitric oxide decomposition will improve the catalysts

performance during the warm-up

period. As it turned out, the added

zirconium lowered the temperature

at which cerium oxide exchanges

oxygen by about 100 degrees Celsius.

Mullins and his collaborators are

now investigating the mechanisms

by which zirconium improves the

catalytic properties of cerium oxide. They are also studying the action of other impurities such as

dysprosium.

ìThe research efforts needed to

optimize the destruction of nitric

oxide in car exhaust are extensive,î

admits Mullins, ìbut the knowledge

that we have gained so far will lead

to more new discoveries.î

 -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - May 17,

2002.]
2 - 13 Chemistry

FUNDING

National Science Foundation, Petroleum

Research Fund, ChevronTexaco, and

Energy Research and Technology

Company.

PUBLICATION

M.G. Wu, M. W. Deem, S.A. Elomari, R.C.

Medrud, S. I. Zones, T. Maesen, C. Kibby, C.

Y. Chen, I. Y. Chan, J. Phys. Chem. B, 106,

264-270 (2002).

FOR MORE INFORMATION

Ronald Medrud, Chevron Research &

Technology Co., Richmond, California

rcme@chevron.com

BEAMLINE

X7A Discovery of a New Molecular Sieve:

M. G. Wu1, M. W. Deem2, S.A. Elomari3, R. C. Medrud3, S. I. Zones3,

T. Maesen3, C. Kibby3, C. Y. Chen3, and I. Y. Chan3

1

Inductive Devices, Pasadena, California; 2Rice University, Houston, Texas; 3ChevronTexaco

Energy Research and Technology Company, Richmond, California

Zeolites, which are primarily made

of silicon and oxygen, have found

widespread use as catalysts, molecular sieves, and ion exchangers.

High-silica zeolites are of particular interest because of their importance in refining and petrochemical applications.

In virtually all instances involving

high-silica zeolites, the crystallization involves complete filling of the

void regions by an organo-cation

guest molecule. Then, the guest

molecule is thermally decomposed,

leaving the ordered void regions of

the zeolite, which can later be studied for catalysis or separation applications.

Our team has found a novel zeolite: Si0.97B0.03O2, designated as

SSZ-55, by using the organo-cation guest molecule shown in Figure 1. A key feature of this molecule is that it has both structural

rigidity, conformational flexibility,

and a positive charge for overall

system neutrality.

It is usually difficult to grow zeolite crystals for single crystal diffraction experiments, although

progress is being made at synchrotron sources to collect data from

micrometer-sized single crystals.

Instead, micrometer-sized crystals

are easily grown and are ideal for

powder diffraction. At NSLS

beamline X7A, which is dedicated

to powder diffraction, our team has

collected high-resolution data on

micrometer-sized zeolite crystals.

The unit cell was determined by

indexing the experimental data

with the commonly used Visser,

Werner, and Louer programs. The

structure was solved using ZEFSAII, a Monte Carlo program designed

specifically for solving tetrahedral

framework structures. The final

structure parameters were obtained by Rietveld refinement with

a widely used program called General Structure Analysis System

(GSAS).

SSZ-55 is tetrahedral (has four

faces) with large pores surrounded

by twelve silicon atoms, also called

ATS. Figure 2 shows projections

of the zeolite molecule in each of

the three crystallographic directions. Of particular interest is a onedimensional channel composed of

12 tetrahedral (T) atoms. The oxygen atoms are omitted for clarity

but are located halfway between

each pair of silicon atoms. (Siliconoxygen-silicon angles are usually

Zeolite SSZ-55

I. Y. Chan C. Kibby

R. C. Medrud S. I. Jones

Scientists at the University of California in Los Angeles, and the

ChevronTexaco Energy Research and Technology Company in Richmond,

California, have discovered a new large-pore zeolite, which is a compound that can be used to separate molecules of various sizes and shapes,

and can act as a sieve by constraining a chemical reaction medium. Due

to their high thermal stability, zeolites are also used as catalysts, both

in the petroleum and the chemical industries.
Science Highlights 2 - 14

Figure 2. Three axial projections of the SSZ-55 structure obtained

from Rietveld refinement. Note that only the silicon atoms are

shown.

Figure 1. Molecule used in the SSZ-55

synthesis: [(1-(-fluorophenyl)

cyclopentyl)-methyl]trimethyl

ammonium ion.

in the range 140 ñ 160 degrees.)

Adsorption experiments with argon

and selected hydrocarbons support

the results of the structure determination. Argon adsorption shows

that the pore opening is 7 ± 1 Å,

which is in good agreement with the

structural values of 6.5 Å x 7.2 Å.

Hydrocarbon adsorption of molecules of various shapes and sizes

reveal that the material has a pore

opening of 12 to 14 rings, in agreement with our structural results.

Though ATS framework structure

has been previously found in a variety of metal-substituted

aluminophosphates (compounds

containing aluminum and phosphate), SSZ-55 is the first discovered high-silica zeolite with an ATS

structure. Also, the synthesis conditions are considerably different

for the two classes of compounds.

SSZ-55 is also interesting in that

the structure does not contain any

five-ring silica subunits, which tend

to predominate in high-silica zeolites. Instead, the structure contains only four-ring and six-ring

subunits.
2 - 15 Chemistry

FUNDING

U.S. Department of Energy,

Office of Basic Energy Sciences

Seitz Materials Research Laboratory

Yeshiva University Research Fund

PUBLICATION

J.A. Rodriguez, J.C. Hanson, A.I. Frenkel,

J.Y. Kim, and M. Perez, J. Am. Chem.

Soc.,124, 346 (2002).

FOR MORE INFORMATION

JosÈ A. Rodriguez, Department of

Chemistry, Brookhaven National Lab.

rodriquez@bnl.gov

BEAMLINE

X7B and X16C

Metal oxides are widely used as catalysts for the conversion of hydrocarbons in the chemical industry and the destruction of the sulfur dioxide and nitric oxide produced during the combustion of fuels in automobiles, factories and power plants. Though these catalysts have been

designed empirically so far, scientists are now starting to understand

how they operate. Using x-rays produced by the National Synchrotron

Light Source, scientists from BNL and Yeshiva University in New York,

have shown a direct oxidation of nickel oxide to nickel without accumulation of any intermediate phase, which may be explained by the presence of oxygen vacancies in the oxide. These results illustrate the complex role played by oxygen vacancies in the oxide reduction process.

Role of Oxygen Vacancies in the Reduction of

Nickel Oxide by Hydrogen

J.A. Rodriguez1, J.C. Hanson1, J.Y. Kim1, and A.I. Frenkel2

1

Brookhaven National Laboratory; 2Yeshiva University, New York

Metal oxides are used as catalysts

in a large variety of commercial

processes for the conversion of

hydrocarbons. Also, due to their

low cost, metal oxides are also used

as supports of many other catalytic

materials. But in most cases, oxides alone are not very good catalysts. So, one method frequently

used to prepare active oxide catalysts is to partially reduce the oxide with hydrogen at elevated temperature.

Reduction of nickel oxide by hydrogen has been the object of numerous studies, because nickel oxide

is a component of many

industrial catalysts and

electromagnetic devices.

So, we decided to look at

the atomic mechanisms

responsible for the reduction of nickel oxide under

temperature ranging from

25 to 400 degrees Celsius.

Such investigations resulted from the successful combination of very intense synchrotron radiation generated by the

NSLS and new parallel

data-collection devices installed at NSLS beamline

X7B.

Experiments at beamline X7B have

previously shown that in situ timeresolved x-ray diffraction (XRD) is

a powerful technique to study oxide reduction. By using XRD and xray absorption techniques, we have

shown that crystal and powder

forms of nickel oxide are directly

reduced to nickel at atmospheric

pressures and elevated temperatures (250 to 350 degrees), but

only after an induction ñ or delay ñ

period.

During the induction period, oxygen vacancies are created within

the crystal of nickel oxide. These

vacancies then favor the adsorption of hydrogen to the oxide and

substantially lower the energy barrier associated with the cleavage

of hydrogen bonds. At the same

time, adsorbed hydrogen can induce the migration of oxygen vacancies from inside the nickel oxide crystal to the surface. By inducing more oxygen vacancies on

the surface, the hydrogen atoms

thus ìautocatalyzeî the oxide reduction process, which becomes

more and more efficient over time.

XRD data collected by studying the

reaction of hydrogen with a nickel

oxide powder at 280 degrees Celsius are shown in

Figure 1. During the first

50 minutes, the intensity

of the diffraction lines for

nickel oxide remains constant (red). Then, these

lines begin to disappear

while lines for metallic

nickel appear (blue), but

no line associated with a

well-ordered intermediate

phase is visible.

By using near-edge and

extended x-ray absorption

fine structure (NEXAFS/

EXAFS) techniques at

Members of the team who conducted the study (from

left to right): Jon Hanson, Anatoly Frenkel, Jose

Rodriguez (lead author) and Jae Kim.
Science Highlights 2 - 16

Figure 1. (Top) Crystal structure of nickel oxide and nickel (nickel: blue; oxygen: red). (Bottom) Time-resolved x-ray

diffraction results for the reaction of a nickel oxide powder with hydrogen at 280 degrees Celsius (red lines: nickel oxide;

blue lines: nickel).

Figure 2. Time-resolved near-edge x-ray absorption fine structure (NEXAFS) data for the reduction of nickel oxide

powder at 280 degrees Celsius under a flow of hydrogen.

beamline X16C, we also observed

a similar induction time. One might

argue that an amorphous phase

(NiOx, 0<x<1), with special chemical properties, might form during

the induction time. This possibility

was ruled out by the NEXAFS data

shown in Figure 2, which reveal

only two compounds after oxide reduction: the produced nickel and

the nickel oxide that was left from

the reaction. (If an amorphous

phase were created, the curve in

Figure 2 would have a different

line shape, corresponding to three

compounds: nickel, nickel oxide

and the amorphous phase.)

Our studies indicate that oxygen

vacancies play a key role in the

reduction of nickel oxide, by generating the necessary sites for the

dissociation of molecular hydrogen

and the subsequent auto-activation

of the oxide catalyst.
2 - 17 Chemistry

FUNDING

University of Massachusetts, Amherst

National Institutes of Health; Division

of Materials Sciences and Division of

Chemical Sciences (U.S. DOE)

PUBLICATION

FOR MORE INFORMATION

BEAMLINE

X9B

Acireductone dioxygenases (ARDs) are enzymes involved in cell cycle

regulation. The ARDs produced by a bacterium called Klebsiella

pneumoniae have been investigated in detail, but the precise function

of one of them, a nickel-containing ARD (Ni-ARD), is unclear. Scientists

from the University of Massachusetts in Amherst and Brandeis University in Waltham, Massachusetts, have examined the structure of the

nickel-containing active site of Ni-ARD, in the presence and absence of

substrate. The results of the study provide the first structural details of

the nickel site in the only known nickel-containing dioxygenase, and

provide insight into substrate binding and the role of nickel in catalyzing

substrate oxidation.

Investigation of the Role of Nickel in the

Regulation of the Cell Cycle

Polyamines are molecules that are

critical for proper regulation of the

cell cycle. Addition of polyamines

to cells accelerates their DNA replication and division, whereas inhibition of polyamine biosynthesis

arrests DNA replication and prevents continuation of the cell cycle.

Methylthioadenosine (MTA) is a

strong inhibitor of polyamine biosynthesis and transmethylation

reactions, so the concentration of

MTA in biological systems is tightly

regulated. This control is achieved

through a regulation mechanism

called the methionine salvage pathway, where MTA is recycled through

a series of reactions that convert it

to methionine.

In Klebsiella pneumoniae, a

bacterium causing pneumonia and urinary tract infection, the pathway has been

investigated in detail, and all

its intermediates have been

identified. One of the intermediates of the pathway,

called acireductone, is catalyzed by two enzymes called

acireductone dioxygenases

(ARDs). The two enzymes

share a common protein and

differ only in the metal ion

present, which is either iron or

nickel.

Reaction of acireductone with ironARD and oxygen produces a precursor of methionine, while reaction of acireductone with nickelARD does not recycle MTA to methionine. The precise function of the

nickel-ARD reaction in K. pneumonia is unclear, and may be considered a shunt in the methionine salvage pathway, aiding in the regulation of methionine. So, we decided to investigate the structure

of the catalytic nickel center in resting nickel-ARD enzyme and the

enzyme-substrate complex, by using x-ray absorption spectroscopy

at beamline X9B of the National

Synchrotron Light Source at

Brookhaven National Laboratory.

We considered the following substrates: acireductone, carbon(14)-

labeled substrates or substrate

analogues, and oxygen(18).

X-ray absorption spectroscopy data

obtained on the enzyme-substrate

complex show that the substrate

binds to the nickel binding site via

two contact sites by displacing two

ligands, at least one of which is a

histidine ligand. These results show

that the nickel-ARD binds to a substrate by activating its oxidation by

oxygen.

Analyses of x-ray absorption nearedge spectroscopy (XANES) and

extended x-ray absorption

fine structure spectroscopy

(EXAFS) data show that the

structure of the nickel binding site in the resting enzyme consists of six nickel

centers with six oxygen or

nitrogen ligands in each center. A schematic representation of a nickel center is

provided in Figure 1.

A comparison of the EXAFS

spectra for resting nickelARD and the nickel-ARD enF. Al-Mjeni, T. Ju, T. C. Pochapsky, and M. J. Maroney

University of Massachusetts, Department of Chemistry

F. Al-Mjeni, T. Ju, T. C. Pochapsky, and M. J.

Maroney, ìXAS Investigation of the

Structure and Function of Ni in

Acireductone Dioxygenase,î Biochemistry, 41, 6761-6769 (2002).

Michael Maroney, Dept. of Chemistry,

Univ. of Massachusetts, Amherst

mmaroney@chem.umass.edu

Faizah Al-Mjeni

(lead author)

Michael Maroney
Science Highlights 2 - 18

Figure 1. Nickel site structure in nickelARD, drawn from information obtained

from x-ray absorption spectroscopy and

nuclear magnetic resonance. The nickel

ion (green) is surrounded by three

histidine residues (purple), a

carboxylate residue (yellow) and two

non-protein ligands (blue squares),

presumably water and/or hydroxide.

Figure 2. Nickel K-edge EXAFS spectra. Fourier-tranformed

(left) and Fourier-filtered (right) spectra of the resting nickelARD (top) and the nickel ARD-substrate (bottom) of Klebsiella

pneumoniae. Data points are represented by red open circles

and the fit by a solid line.

-6

-4

-2

0

2

4

6

2 4 6 8 10 12

10

8

6

4

2

0

0 2 4 6 8

10

8

6

4

2

0

0 2 4 6 8

-6

-4

-2

0

2

4

6

2 4 6 8 10 12

FT Magnitude (x 102

) FT Magnitude (x 102

)

k(Å-1) r(Å)

zyme-substrate complex (Figure

2, top-right and bottom-right spectra) reveal changes implying that

the substrate binds to the nickel

site. One of these changes is a dramatic decrease in the intensity of

features at a distance of 3 to 4

angstroms, which we believe are

due to the presence of histidine

imidazole ligands, suggesting that

one or more histidine ligands are

displaced when a substrate binds

to nickel-ARD.

Dioxygenases are known to operate by two distinct types of mechanism: One involves a redox active

metal center to activate oxygen to

oxidize the substrate. The second

mechanism involves activation of

the substrate via coordination to

the metal center in order to activate it toward oxidation by

dioxygen. This latter mechanism,

where the metal center need not

be redox active, is supported by the

XAS results.

We are currently investigating the

use of nuclear magnetic resonance

methods to characterize in more

detail metal-bound substrate species in iron- and nickel-ARDs, and

to understand better the differences between the differing activities of these two enzymes.
2 - 19 Chemistry

FUNDING

Institut National des Sciences de líUnivers

(INSU), France; U.S. DOE, Division of

Materials Sciences and Division of

Chemical Sciences; National Science

Foundation; and Center for Biological and

Environmental Nanotechnology (CBEN),

Rice University

PUBLICATION

J. Rose, et al. ìSynthesis and Characterization of Carboxylate-FeOOH Nanoparticles (Ferroxanes) and FerroxaneDerived Ceramics,î Chem. Mater, 14, 621-

628 (2002).

FOR MORE INFORMATION

JÈrÙme Rose, CEREGE

rose@cerege.fr

BEAMLINE

X23A2

Ceramic oxides are widely used in

industry (for example as catalysts,

paint pigments, medical supplies,

chemical sorbents, and magnetic

products), so new synthetic methods to produce iron oxide are constantly developed. Two common

processes are currently used to

produce oxide ceramics: powder

processing and sol-gel. But powder processing ñ which is typically

used to produce bulk quantities of

the ceramic ñ involves potentially

toxic agents, such as binders and

solvents, and the sol-gel process

may yield environmentally harmful products such as strong acids,

binders, and solvents.

It is thus desirable to develop new

synthetic methodologies to overcome the drawbacks of current processing techniques. We have developed a new approach for the

synthesis of iron oxide ceramics

based upon the reaction of large

minerals with carboxylic acids. A

new iron precursor for iron-ceramics, called carboxylate-ferroxane

(carboxylate-FeOOH), was prepared by reacting lepidocrocite (γFeOOH), a layered mineral, with

acetic acid (AA) in water.

The atomic environment of iron

Synthesis and Characterization of CarboxylateScientists from the Univ. of Aix-Marseille in France, Rice Univ. in Houston, and the Savannah River Ecology Lab. in Aiken, S.C., have shown

that the reaction between a natural iron mineral named lepidocrocite (γFeOOH) and acetic acid (C2H4O2, denoted AA) in water results in the

formation of carboxylate-FeOOH nanoparticles called ferroxane-AA. Upon

thermolysis (cleavage of atomic bonds by exposure to high temperature), the nanoparticles evolve to homogeneous iron-metal oxides. A

low firing temperature for conversion to ceramic as well as the use of

environmentally benign reagents suggest that this process for creating

ferroxane-derived ceramics should have minimal environmental impact.

J. Rose1, M. M. Cortalezzi2, A. R. Barron2, M. R. Wiesner2, A. Masion3, S.

Moustier3, J.-Y. Bottero3 and P. Bertsch3

1

Centre EuropÈen de Recherche et díEnseignement des GÈosciences de líEnvironnement

(CEREGE), Aix en Provence, France, 2

Center for Biological and Environmental

Nanotechnology (CBEN), Rice Univ.; 3Savannah River Ecology Lab.

within the ferroxane was determined using iron K-edge x-ray absorption spectroscopy (XAS) of the

dehydrated samples. The

ferroxanes were also doped with

zirconium, the structural site of

FeOOH Nanoparticles (Ferroxanes) and

Ferroxane-Derived Ceramics

Members of the team at the University of Aix-Marseille in France (from

left to right): Jean-Yves Bottero, StÈphane Moustier, Armand Masion,

and JÈrÙme Rose (lead author).

Members of the Rice University team (from left to right): Mark Wiesner,

Maria Cortalezzi, and Andrew Barron.
Science Highlights 2 - 20

Figure 1. (A) Atomic force microscopy (AFM) image of the texture and structure of ferroxane nanoparticles on a metallic

surface. Apparent sizes of four ferroxanes are shown (116, 84, 92, and 84 nanometers). (B) Size of the nanodomains of

each ferroxane. (C) Atomic structure of the nanodomains (brown: iron octahedra; red: oxygen atoms; green: zirconium

site for doped sample).

which was characterized at the zirconium K-edge. XAS spectra were

recorded at NSLS beamline X23A2.

The structure and texture of the

ferroxane were characterized by

combining spectroscopic methods

(Fourier-Transform Infrared (FTIR),

XAS, x-ray diffraction (XRD), and

light scattering), microscopic methods (atomic force microscopy

(AFM) and scanning electron microscopy (SEM)) and gas adsorption data.

The current results (Figure 1)

show that AA may cleave and break

the lepidocrocite, yielding a new

product: ferroxane. Ferroxanes are

300 nanometers (nm) in size and

are composed of nanodomains of

20 nm in size with a γ-FeOOH structure. Each ferroxane particle is

composed of a lepidocrocite core,

on which AA is chemically

adsorbed, as revealed by the spectroscopic techniques.

Thermolysis (cleavage of atomic

bonds by exposure to high temperature) of the ferroxane-AA

yields iron ceramic with the crystallographic structure of hematite.

The specific surface area does not

increase from the initial FeOOH

mineral to the ferroxane-AA and

the iron-ceramic, while the pore

size distribution becomes monodisperse and the pore size diameter

decreases from 55 to 12 and 13

nanometers after firing.

The ferroxane-AA was successfully

doped with zirconium, which was

incorporated within the structure of

the ferroxane-AA. After firing zirconium-doped ferroxane-AA

samples, a mixed iron-zirconium

oxide was formed.

Key to this work was the development of nanoparticles using a

ìgreenî chemistry approach. Also,

the ferroxanes are indefinitely

stable under ambient conditions

and are adaptable to a wide range

of processing techniques.

We are currently testing the possibility of using the ferroxanes for

different applications such as the

synthesis of iron membranes and

the development of new catalytic

materials.

A. B. C.
2 - 21 Chemistry

FUNDING

U.S. Department of Energy

National Science Foundation

PUBLICATION

A.M. Argo, J.F. Odzak, F. S. Lai, and B.C.

Gates, ìObservation of Ligand Effects

during Alkene Hydrogenation on

Supported Metal Clusters,î Nature, 415,

623 (2002).

FOR MORE INFORMATION

Bruce Gates, Dept. of Chemical Engineering and Materials Science, Univ. of

California, Davis

bcgates@ucdavis.edu

BEAMLINE

X11A

Metals in catalysts used in petroleum refining or automobile exhaust conversion usually are in the

form of clusters, each a few billionths of a meter in size, attached

to a support. Because the clusters

are so small, a large fraction of the

atoms on the cluster surface is exposed, thus increasing the rates of

chemical reactions. But such cluster-based catalysts are

not well understood because they are made of

particles of varying

sizes. Scientists have

developed structurally

simple models, usually

of single crystals, but

such models do not provide information about

the supportís role in a

chemical reaction.

We prepared nearly uniform metal nanoclusters on supports, identified the catalytic clusters and their interactions with the support

by using extended x-ray

absorption fine structure (EXAFS) spectroscopy, and identified the

reactant-derived

ligands by applying inA Catalyst in Action: Structure and Bonding of

Supported Iridium Nanoclusters During Propene

Hydrogenation Catalysis Determined by EXAFS

and Infrared Spectroscopies

A. M. Argo, J. F. Odzak, and B. C. Gates

Dept. of Chemical Engineering and Materials Science, Univ. of California, Davis, CA

The structures of catalysts ñ ranging from molecular complexes and

enzymes to clusters dispersed on supports ñ depend on the conditions

under which they are used. So, the most incisive determinations of

catalyst structures require techniques characterizing functioning catalysts. Scientists at the University of California, Davis have used X-ray

absorption spectroscopy in combination with infrared spectroscopy to

investigate supported metal cluster catalysts as they functioned, revealing the structure of the catalyst, consisting of four iridium atoms

(Ir4), and the roles of the ligands, including the support. This is the first

characterization of a solid catalyst, elucidating the interplay of the support and reactant-derived ligands through their bonding with Ir4.

frared spectroscopy. The EXAFS

spectroscopy techniques were developed at NSLS beamline X11A.

We investigated the reaction of propene with molecular hydrogen (H2)

to form propane, catalyzed by clusters consisting of four iridium atoms (Ir4) dispersed on porous

γ-Al2O3 or MgO. The catalytic activity of Ir4 depends on the support. Replacement of the MgO support with γ-Al2O3 boosts the catalytic activity tenfold.

When the catalyst attaches to propene or H2 alone, we observed no

significant changes in the iridiumiridium or iridium-oxygen distances. But during a catalytic reaction, the iridium-iridium and the longer,

non-bonding iridiumoxygen distances exceeded the corresponding distances

observed under noncatalytic conditions.

We attribute the distance elongations to

reaction intermediates

bonded to Ir4.

The two supports have

different characteristics that affect the

electronic properties of

the clusters, which in

turn affect the interactions of the clusters

with the ligands

formed from the reactants. So, the support

influences the reactivities of the reactant-deAuthors (clockwise from left): Andrew Argo, Josip Osdak, and

Bruce Gates.
Science Highlights 2 - 22

Figure 1. Schematic representation of the reaction of propene with hydrogen on MgO-supported Ir4 catalyst. The structural

changes shown were determined by extended x-ray absorption fine structure (EXAFS) spectroscopy of the working catalyst.

rived ligands ñ determining which

ones are observed during catalysis

ñ and thus affects the rate of the

catalytic reaction.

Our observations are consistent

with the reaction mechanism

shown schematically in Figure 1.

In addition to electronic effects

caused by the support, geometric

properties of the clusters distinguish them from other metal catalysts. The smallness of the clusters

limits the structures that can be

bonded to them, thereby affecting

the reactivity.

The electronic and geometric effects of the ligands are analogous

to those known in molecular and

enzymatic catalysis. Our results

bolster theoretical cluster models

that incorporate the support, and

indicate new opportunities for tuning the catalytic properties of smallsupported clusters by changing the

nature of the support. None of the

understanding emerging from this

work would have been possible

without the use X-ray absorption

spectroscopy and its application to

working catalysts.
Condensed

Matter Physics
2 - 23 Condensed Matter Physics

Origin of Superconductivity in Fullerenes Still a Mystery

Structure of a fullerene crystal (blue) with chloroform

molecules (green/purple) inserted within the lattice. Although

the structure was expected to be cubic, Dinnebier and his

coworkers found that it was, in fact, hexagonal, as shown in

the figure.

Soccer-ball-shaped molecules

called fullerenes can carry electricity with no energy loss ñ a phenomenon called superconductivity

ñ at temperatures below -387 degrees Fahrenheit. To increase this

temperature, and thus make

fullerenesí use more convenient for

applications in electronics, drug delivery, and nanotechnology, scientists have long assumed that they

simply needed to introduce larger

and larger atoms inside fullerene

compounds.

In the April 5, 2002 issue of

Science, however, scientists

working at the NSLS report

an unexpected result:

When they added molecules of bromoform and

chloroform to a fullerene

compound, the resulting

compound changed its

structure.

This result contradicts a

widely held assumption that

the structure remains the same

in both pure and ìmixedî fullerene

compounds, and paves the way to

a new understanding of

how superconductivity

works in these compounds.

ìThe theory of superconductivity in fullerenes is still

too simple,î says Robert

Dinnebier, a physicist at the Max

Planck Institute for the Physics of

Solids in Stuttgart, Germany, one

of the world leading labs in materials science. ìOur finding means

that the increase in temperature

seems to be due to other causes

than just an increase in spacing

between the fullerene molecules.î

Dinnebier and his colleagues came

upon this new result while attempting to understand findings published a month earlier in Science.

A team of physicists led by physicist Hendrik Schoen, of both Bell

Laboratories in Murray Hill, New

Jersey and the University of

Konstanz in Germany, had, for the

first time, reported that when chloroform and bromoform were added

to fullerene compounds, their superconducting temperature increased dramatically.

ìWhen this work was published, we

immediately thought it would be

very interesting to look at the structure,î Dinnebier says. Detailed

structural studies of the spacing

between fullerenes might explain

the increase in temperature, the

scientists assumed. ìWithin two

weeks, we prepared the material

and sent it to the NSLS,î Dinnebier

says.

At the NSLS, Dinnebierís collaborators Peter Stephens, a physicist

at the State University of New York

at Stony Brook, and his doctoral

student, Ashfia Huq, set up an experiment to look at the structure

of the chromoform- and bromoform-based fullerenes.

ìWhen Robert [Dinnebier] told me

that the material would be available, I was very excited,î Stephens

says. ìWe had to act quickly, because this was just before the Light

Source would shut down for two

months for routine maintenance.î

To reveal the materialís crystalline structure, the scientists used a technique

called powder x-ray crystallography. They projected x-rays produced

by the NSLS toward a

powder of tiny crystals of

the compound. Then,

they determined its structure by looking at how the

x-rays scattered off the

crystals. In one week, the scientists had produced the necessary data and started analyzing

them.

By measuring the distances between the

fullerene molecules in

three directions (updown, left-right, and forward-backward), the researchers found that the expansion

of the molecules due to the bromoform or chloroform mainly takes

place in one direction, instead of

three directions, as predicted. Surprised at first, the scientists later

realized that the structure of the

compounds was different from

what was theoretically predicted.

In a fullerene compound, the molecules form a series of connected

cubes in three directions. The molecules are on the corners of each
Feature Articles 2 - 24

cube, and at the center of the

cubeís faces.

Schoenís group expected that when

bromoform or chloroform molecules are inserted inside a

fullerene compound, they would sit

in between the fullerene molecules.

In this way, the fullerene molecules

would be pushed apart similarly in

the three directions, Dinnebier explains.

The new results show that the

fullerene compounds with chloroform or bromoform were no longer

cubic. Instead, the fullerene molecules form six-sided hexagonal

shapes. The compound is made of

parallel planes, each containing a

series of connected hexagons. ìThe

chloroform and bromoform molecules sit in between the planes,

pushing the fullerene molecules

apart only in the direction perpendicular to the planes,î Dinnebier

says.

While these results give a clearer

picture of how a fullerene compound can be modified by adding

chloroform or bromoform, they still

do not provide answers to what

causes the increase of the superconducting temperature. One possibility is that when chloroform or

bromoform molecules are added to

the fullerene compound, their electrons add to the ones already existing in the compound. The collective motion of all the electrons

then creates heat that increases

the temperature.

According to the theory, the number of electrons would have to increase by 25 to 35 percent to explain the measured superconducting temperature. However, theoretical physicist Olle Gunnarsson,

a member of the Stuttgart team,

showed that, in a hexagonal structure, the number of electrons increases by, at most, 10 percent.

Another possibility, suggested by

Dinnebier and his colleagues in

their article, is that the chloroform

and bromoform molecules may

play a role through interactions

between their electrons, but this

hypothesis has not yet been tested.

ìUnderstanding the causes of superconductivity and the origin of

the temperature below which it

operates are still elusive,î Stephens

says. ìBut these results form the

basis for uncovering how fullerenebased compounds generate superconductivity at the atomic level.î

ìThis kind of research is a beautiful advertisement for the way the

NSLS works,î he adds. ìAt the

NSLS, like many other synchrotron

sources, it is curiosity-driven scientists, not committees, that make

the decisions to schedule most of

the experiments. We owe the success of this work to this well-established culture at the NSLS.î

BEAMLINE

X3B1

PUBLICATION

Robert E. Dinnebier, et al., ìStructure of Haloform Intercalated C60

and Its Influence on Superconductive Properties,î Science, 296, 109

(2002). -Patrice Pages
2 - 25 Condensed Matter Physics

Research by physicists at the NSLS

provides new insight into why some

materials made of stacks of metallic planes are conductors in the direction of the planes and are insulators in the direction perpendicular to the planes. Such behavior is

in marked contradiction with scientistsí traditional understanding of

metallic conductivity, where the

electrical current is carried by electrons in every direction. Understanding how materials that are

both conducting and insulating will

help scientists gain new insight into superconductors

ñ materials that conduct

electricity with no energy

loss.

Scientists have suspected

that the dual conductinginsulating property is due

to electrons interacting so

strongly with each other

that they do not move individually, but collectively,

to carry the current within

the planes. But there has

been no evidence of such

interactions ñ until now.

ìA material that is both conducting and insulating is

quite intriguing,î says Brookhaven

physicist Tonica Valla, the lead author of the study, which appears in

the June 6, 2002 issue of Nature.

ìSuch a dual behavior has puzzled

physicists for several years. And

though theoretical explanations

have been suggested, we now

show for the first time that the

strength of the interactions between excited electrons influences

their behavior.î

Valla and his collaborators from

Brookhaven, the University of Connecticut in Storrs, Princeton University, and Osaka University in

Japan studied two different conConducting-Insulating Materials Reveal Their Secrets

ducting-insulating materials, and

showed that electrons that were

confined in the planes at high temperatures are able to move between the planes at lower temperatures, allowing the material to behave more like a metal.

The ìcriticalî temperature at which

the change occurs ranges between

-100 and -300 degrees Fahrenheit,

depending on the material.

ìThese planes act like trains and

electrons like passengers in the

trains,î says study coauthor Peter

Johnson, a Brookhaven physicist.

ìAt high temperatures, the electrons are bound together in the

planes like passengers inside moving trains. Then, below the critical

temperature, the electrons are not

bound anymore and start moving

around in the same way as passengers leave a stopped train.î

To examine the interactions between the electrons, the scientists

used extremely intense ultraviolet

light generated by the NSLS. They

looked at how the light excites the

electrons in each of the three materials, and used a method called

angle-resolved photoemission

spectroscopy (ARPES) to accurately

measure the intensity of the light

emitted by the electrons as a function of their energy. The resulting

ARPES spectrum was determined

for various temperatures.

Below the critical temperature, a

signal started to appear in the spectrum. Weak at first, the signal became more apparent as the temperature decreased. ìThis signal is

the telltale evidence of individual electrons,î Valla

says. ìTheorists had predicted the existence of

such a signal, but nobody

had observed it before.î

The results of this study

promise to provide further

insight into how superconductors conduct electricity

without heat dissipation

when they are cooled below a certain temperature.

In particular, the cause of

high-temperature superconductors, with critical

temperatures ranging

from -396 to -216 degrees

Fahrenheit, remains mysterious, but is assumed to be due

to strong interactions between

electrons.

The new study also gives insight

into materials with new electrical

and magnetic properties, expected

to arise from strong interactions

between electrons. ìWe expect to

see dramatic new results and applications stemming from the study

of materials with strongly-interacting electrons,î Johnson says.

Physicists Tonica Valla (left) and Peter Johnson at the

NSLS beamline U13, where they study the properties of

conducting/insulating materials.

-Patrice Pages
Feature Articles 2 - 26

New insight into the superconductivity of magnesium diboride

(MgB2) has been recently revealed

by a team of scientists from BNL,

the National Institute of Standards

& Technology (NIST), and the University of Oslo in Norway. The findings appear in the June 17, 2002

issue of Physical Review Letters.

The new information about MgB2,

an unusual superconductor discovered only last year, promises more

understanding of superconductivity ñ the ability of some materials

to conduct electricity without losing energy ñ which could lead to

improved magnetic resonance imaging, more efficient electric power

transmission, and smaller, more

powerful electronic devices.

ìScientists usually assume that superconductivity arises from electrons coupling in pairs,î said Yimei

Zhu of BNLís Energy Sciences &

Technology Department, lead author of the study. ìThough this is

the case for most superconductors,

it has not been shown yet how electrons contribute to superconductivity in magnesium diboride.î Therefore, the team decided to investigate this through research supported by DOE and DOC.

Since the discovery of superconductivity in MgB2, BNL theoretical

scientists, led by physicists James

Davenport, Energy, Environment,

& National Security Directorate,

and Guenter Schneider, Physics

Department, made extensive calculations involving interactions between electrons or between electron ìholes,î which are empty locations that could be filled by electrons.

ìSuperconductivity in MgB2 is exBNL, NIST, Norway Gain New Insight into the Superconductivity

of MgB2

x-rays enter the sample and are

absorbed by the electrons inside it.

In this experiment, the electrons,

which are ejected out of their original positions, are tracked in a

unique x-ray detector, designed

and built by NIST physicist Daniel

Fischer and his team.

ìWhen the ejected electrons fall

into the holes, they reveal the number and density of the holes in the

sample,î said Fischer, who has

worked with the x-ray absorption

technique for the last 18 years at

the NSLS.

The second technique uses stateof-the-art transmission electron

microscopes (TEMs) at BNL. Unlike

optical microscopes, which use visible light, electron microscopes

project electrons toward the

sample. These electrons transfer

some of their energy to electrons

in the sample, which bump around

the sample atoms and reveal the

pected to arise from interactions

between holes,î says BNL physicist

Arnold Moodenbaugh, a member of

the team. ìBecause MgB2 is made

of alternating planes of boron and

magnesium atoms aligned parallel

to one another, these holes are

expected to interact more easily

within the planes than between

adjacent planes.î

ìCompared to other superconductors, MgB2 has a relatively simple

structure,î says Johan Tafto, a

physicist at the University of Oslo

and another team member. ìWe

hoped to get more insight into superconductivity by focusing on a

simple compound rather than on

more complex ones.î

To test the theoretical predictions

about MgB2, the researchers used

two complementary techniques: xray absorption spectroscopy and

electron-energy-loss spectroscopy.

In the first technique, very intense

Near the NIST/Dow beamline U7A at the NSLS, where part of the MgB2 study was

conducted, are team members Daniel Fischer, Yimei Zhu, Genda Gu, Arnold

Moodenbaugh (back), Johan Tafto, Tom Vogt and James Davenport. Absent from

the photo are team members Guenter Schneider and Qiang Li.
2 - 27 Condensed Matter Physics

positions of electronic holes in the

sample.

ìWe needed to use both techniques

because they complement each

other so well,î Zhu said. ìThey lead

to a very accurate determination

of the distribution and number of

electron holes in MgB2.î The leader

of BNLís TEM group at the Advanced

Electron Microscopy Facility, Zhu

has been investigating the electronic structure of materials at the

A plane of magnesium atoms (white spheres) above a

plane of boron atoms (grey spheres) in MgB2, as seen

by the transmission electron microscope used in the

study. The embedded image (top left) is a model of the

structure, showing the expected positions of the atoms

and the distance between two magnesium planes.

nanoscale (one billionth of a meter)

for the last 20 years.

By showing that interactions between holes in the boron planes do

occur in MgB2, and that superconductivity stems from such interactions, the scientists showed that

results from both techniques agree

with the theoretical predictions.

Said Tafto, ìAs we gain more understanding of the properties of

MgB2 at the atomic level, I am confident that, in the near future, we

will be able to relate them to macroscopic properties such as superconductivity - and maybe explain

the origin of superconductivity in

general.î

An illustration of the distribution of electrons between

boron and magnesium atoms. Electrons cluster around

the boron atoms (yellow peaks) and move away from

the magnesium atoms (orange valleys).

-Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - June 21,

2002.]
Feature Articles 2 - 28

Many techniques are currently

available to investigate electronic

properties ñ such as conductivity

and magnetism ñ of solids, but for

materials made up of different

chemical elements, the contributions of the electronic properties of

the atoms of each element are difficult to distinguish. Now, a team

of scientists has perfected a new

technique that does just that.

The scientists have been working

on the technique, called site-specific x-ray photoelectron spectroscopy, for the past two years, and

have recently used it to investigate

the electronic properties of oxygen

and titanium atoms in rutile, a mineral made of titanium dioxide usually with a little iron, and used to

accelerate chemical reactions. The

results of the study, reported in the

August 12, 2002 issue of Physical

Review Letters, represent the first

experimental application of the

technique to a metal oxide, thus

paving the way to understanding

the properties of more complex

Scientists Create ëLight Tweezersí to Study the Electronic

Properties of Solids

metal oxides used in the chemical

and electronics industry.

ìOur technique can unambiguously

determine the individual contributions of either the titanium or the

oxygen atoms to the electronic

structure of rutile,î says physicist

Joseph Woicik, of the National Institute of Standards and Technology (NIST) in Gaithersburg, Maryland, and the lead author of the

study. ìIn contrast, other techniques describe the electronic

structure of rutile as a whole, which

does not say much about how titanium and oxygen atoms interact

with each other.î

Picking Different Atoms

With Optical ìTweezersî

The new technique, which combines two widely used techniques,

called photoelectron spectroscopy

and x-ray diffraction, works as follows: Very intense x-rays are first

projected towards the material and

then deflected by the atomic planes

of the material, creating ìdiffractedî x-rays. When the incident

and diffracted x-ray waves combine, they form a standing wave,

which is used to excite electrons

inside the material. The period of

the standing wave, which is the distance between two crests, can be

made equal to the distance between two atoms of a given element. As a result, the crests of the

wave selectively excite the electrons of the atoms of a given element, but not the electrons of the

atoms of other elements. The

crests of the standing wave can

then be moved in a controlled fashion, thereby allowing them to

stimulate electrons of the other elementsí atoms at will.

To study the electronic properties

of titanium and oxygen atoms in

rutile, Woicik and his colleagues

used x-rays generated by the

NSLS.

ìBecause the waves have the same

period as the inter-atomic distance,

we can selectively excite either the

titanium atoms or the oxygen atoms,î Woicik says, ìand when one

of these atoms is excited, all the

other atoms of the same element

are excited at once.

ìThe crests of the standing wave

act like tweezers that reach in and

pick out electrons,î Woicik says.

ìThe advantage is that you know

that the electrons you are studying are coming from either the titanium or the oxygen, but not

both.î

The scientists analyzed the energy

of the ejected electrons to gain information about the electronsí positions and energies in the crystal

before the electrons were excited.

At beamline X24A (from left to right): Physicist Joseph Woicik

(lead author), beamline technical support Barry Karlin and

physicist Lonny Berman (co-author). (courtesy of Daniel Fischer,

NIST).
2 - 29 Condensed Matter Physics

The analysis was performed with a

state-of-the-art device called an

electron analyzer, and ultra-high

vacuum tools specially designed

and built by scientists from the

University of Rhode Island in

Kingston, the NSLS, and NIST,

working at NSLS beamline X24A.

Covalent Bonds and

Electric Insulation

By closely looking at the positions

of the electrons, Woicik and his

colleagues found that the binding

of the titanium and oxygen atoms

does not follow the more conventional ionic picture, in which the

electrons responsible for the binding hover around oxygen atoms but

not titanium atoms. The new study

shows that, instead, titanium and

oxygen atoms share their electrons, making ìcovalentî bonds.

ìWe were surprised to notice such

a substantial electron density coming from the titanium atoms,î

Woicik says. ìThis means that electrons are present around the titanium atoms, which shows that the

bonding is covalent.î

Figure 1: Crystallographic structure of rutile. Titanium atoms are represented

by large spheres and oxygen atoms by small spheres.

Figure 2: Comparison of theoretical

and experimental densities of states of

electrons surrounding the titanium (top)

and oxygen (down) atoms. The

experimental curves, which were

obtained from the site-specific x-ray

photoelectron spectroscopy technique,

agree nicely with the theoretical curves,

attesting for the ability of the technique

to act as ìlight tweezers,î picking out

either the titanium or oxygen atoms.

The researchers also examined the

positions of electrons responsible

for the conducting or insulating

properties of a solid. In the case of

rutile, they found that the electrons

with the highest energies are not

jumping between the atoms, as

would be expected in a conductor,

but are localized around the oxygen atoms, justifying that rutile is

an insulator.

Unexpected Experimental

Results

The new experimental results

nicely agree with theoretical expectations. But this agreement came

as a surprise. Last year, Woicik and

his colleagues were testing their

technique on copper when they discovered that ìvalenceî electrons,

which are peripheral to the nuclei,

displayed emission patterns similar to ìcoreî electrons, which are

localized close to the nuclei.

ìWe could not believe what we were

seeing,î Woicik says. ìBecause valence electrons are free to roam in

between atoms, there was no reason that their emission patterns

would be the same as those of core

electrons.î

Half convinced that their presumptions might be incomplete, the scientists considered more carefully

the nature of the electron waves

within the crystal. ìOur presumptions were wrong,î Woicik says.

ìOnly when the valence electrons

are near the cores can they be excited by the x-rays.î

These observations demonstrated

that the scientists need to consider

only the contributions from the individual atoms. ìThe technique

truly works like tweezers that only

reach in and grab the electrons in

the immediate vicinity of each

atom,î Woicik says. ìThis was the
Feature Articles 2 - 30

-Patrice Pages

most startling observation that I

have ever made in 13 years working in this field.î

More Results to Follow

The researchers are now interested

in applying their technique to more

complex metal oxides than rutile,

including materials in which electrons interact collectively, a phenomenon responsible for superconductivity ñ electrical conductivity

without energy loss below a certain temperature. The technique

could also be used to shed light on

the magnetic properties of materials by looking at the magnetic properties of individual nuclei and electrons.

ìThe beauty of our technique is that

it can unravel the electronic structure of simple metal oxides in a way

similar to the way you peel an onion,î Woicik says. ìBy looking at

how electrons interact with each

other, you can then make more

sense of the electronic properties

of more complex metal oxides and

possibly address intriguing phenomena such as high-temperature

superconductivity and metal-insulator transitions.î

BEAMLINE

X24A

PUBLICATION

J.C. Woicik, E.J. Nelson, L. Kronik,

M. Jain, J.R. Chelikowsky, D.

Heskett, L.E. Berman, and G.S.

Herman, ìHybridization and BondOrbital Components in Site-Specific

X-Ray Photoelectron Spectra of

Rutile TiO2î, Phys. Rev. Lett. 89,

077401 (2002).
2 - 31 Condensed Matter Physics

FUNDING

Department of Energy (DOE)

The A. P. Sloan Foundation

PUBLICATION

Z. Yusof et al., "Quasiparticle Liquid in the

Highly Overdoped Bi2

Sr2CaCuO8+d",

Physical Review Letters 88, 167006 (2002).

FOR MORE INFORMATION

Zikri Yusof

Physics Department

University of Connecticut, Storrs, CT.

yusof@bnl.gov

BEAMLINE

U13UB

Quasiparticles Refuse to Go Away in HighZ. Yusof1

, B.O. Wells1, T. Valla2, A.V. Fedorov2, P.D. Johnson2, Q. Li2, C.

Kendziora3, Sha Jian4, and D.G. Hinks4

1

University of Connecticut, Storrs; 2Brookhaven National Laboratory; 3Naval Research

Laboratory, Washington, D.C.; 4

Argonne National Laboratory, Illinois

Scientists working at NSLS beamline U13UB have shown that provided

new insight into the properties of overdoped cuprates (bismuth-strontium-copper-oxides). The researchers found that while underdoped

cuprates have exotic properties, overdoped cuprates behave more like

regular metals.

Fifteen years after the discovery of

cuprate (bismuth-strontium-copper-oxide) superconductors

(1986), the origin of superconductivity in these materials is still unknown, and scientists are still investigating the nature and behavior of the charge carriers in these

materials. One of the most studied

of these compounds is

Bi2Sr2CaCu2O8+δ , also called Bi2212,

which has provided considerable insight - as well as new puzzles - on

the origin of high-temperature superconductivity.

Cuprates share a set of generic fea- tures. These compounds become

superconductors only when they

are doped with electrons or holes.

Undoped, they are antiferromagnetic insulators. As they are doped

either with holes or electrons, they

evolve first into a strange metal and

eventually become superconducting with increasing critical temperature Tc until this temperature

reaches a maximum value at what

is known as optimal doping. Increasing the doping level beyond

this point causes Tc to drop again

(Figure 1). A doping level below

the optimum value is known as

underdoping, while that above the

optimum value is known as

overdoping.

The underdoped and optimallydoped superconductors have a

number of unusual properties, especially in the normal state (above

Tc

). One puzzling property is the

apparent absence of "quasiparticles", entities that are defined in

Landau's Fermi Liquid theory. This

theory has successfully described

the properties of ordinary metals,

semiconductors and conventional

superconductors (discovered before 1986), but cuprates, especially

in their normal state, appear to

defy explanation with this theory.

Samples of overdoped cuprates

have been studied using angle-resolved photoemission spectroscopy

Temperature Superconductors

Figure 1. Generic phase diagram of

high-Tc superconductors.

(From left) Peter Johnson, Tonica Valla, Zikri Yusof, and Barry Wells
Science Highlights 2 - 32

(ARPES), which is a more sophisticated version of the familiar photoelectric effect. In ARPES, the outgoing photoelectrons are collected

by an electron analyzer that allows

us to obtain the energy and momentum distributions of these electrons. The presence of a quasiparticle gives a sharp peak in the

ARPES spectrum.

We found that the superconducting state has quasiparticles at all

doping levels but they persist to the

normal state only for the overdoped

compound (Figure 2). We also established that while underdoped

cuprates have exotic charge transport, the overdoped cuprates have

more familiar quasiparticle physics - closer to a regular metal like

copper. The next step is to understand how the material evolves

from one form to another, either

through a gradual crossover or a

sharp phase transition.

Figure 2. Energy distribution of photoelectrons. (a) Optimally doped

superconductor with Tc=91K. The sharp peak in the spectra, representing welldefined quasiparticles, is not detected above Tc [Fedorov et al. PRL 82, 2179

(1999)]. (b) Overdoped superconductor with Tc=51K. Sharp peak (quasiparticles)

exists well above Tc.

Energy (eV)

Intensity (arb. units)

Energy (eV)
2 - 33 Condensed Matter Physics

FUNDING

Office of Basic Energy Research

U.S. Department of Energy

PUBLICATION

Q. Qian,T. A. Tyson, C.-C. Kao, M. Croft,

and A. Yu. Ignatov, ìLocal Magnetic

Ordering in La1-xCax

MnO3 Determined by

Spin-Polarized X-ray Absorption Spectroscopy,î App. Phys. Lett. 80, 17, 3141 (2002).

FOR MORE INFORMATION

Trevor Tyson, Assistant Professor,

Department of Physics, New Jersey

Institute of Technology, Newark, NJ

Tyson@admin.njit.edu

BEAMLINE

X21

In the transition metal oxide La1-xCaxMnO3 (with 0<x<1), electrical conductivity is strongly influenced by external magnetic fields, making this

material an exceptionally good candidate for a new generation of magnetic sensors that may significantly improve magnetic data storage. To

probe the local spin arrangement in transition metal oxides, we have

developed a method to directly assess the local magnetic ordering about

specific metal atoms. This method promises to lead to a better understanding of magnetism in magnetic oxides and to assist in improving

theoretical models of correlated electron systems.

Probing Local Magnetic Order in Transition

Metal Oxides

Q. Qian1, T. A. Tyson1, C.-C. Kao2, M. Croft3 and A. Yu. Ignatov1

1

New Jersey Institute of Technology; 2Brookhaven National Laboratory, NSLS; 3Rutgers

University

Intriguing phenomena such as

high-temperature superconductivity (electrical conductivity without

resistance) and colossal magnetoresistance (change in electrical

resistance due to the presence of

a magnetic field) have stimulated

renewed interest in the physics of

transition metal oxides based on

perovskite (CaTiO3), by using techniques such as x-ray absorption

spectroscopy (XAS) and x-ray

emission spectroscopy (XES).

High resolution XAS work has provided evidence of intriguing temperature dependencies of the manganese K-XAS preedges of La1-xCaxMnO3

materials which accompany changes upon

crossing phase boundaries involving combinations of insulating, paramagnetic, antiferromagnetic, ferromagnetic,

and charge-orbital ordered phases. But these

interphase changes are

not well understood.

Consequently, we used

a powerful combination

of XAS and XES, called

spin-polarized x-ray absorption near edge

spectroscopy (SPXANES), to extract spin-polarized x-ray absorption spectra and integrate the results into a model which is sensitive to local magnetic order.

SPXANES is based on energy resolving the 3p to 1s transition (Kfl

emission) and measuring the emission from the main or satellite lines

of the spectra as a function of the

incident x-ray energy. Previous

studies focused on the nature of

the splitting between spin up and

spin down channels in the main

line, but no emphasis was made

on the pre-edge region and on the

temperature-dependent changes in

SPXANES.

Manganese SPXANES measurements were performed at beamline

X21 of the National Synchrotron

Light Source. SPXANES spectra

were collected by monitoring the

Kfl fluorescence yield at two energies, specific to spin up and down

final states, while the incident energy across the near-edge region

was scanned. Measurements were

performed for x = 0, 0.3, 0.5, and

1 (corresponding to LaMnO3,

La0.7Ca0.3MnO3, La0.5Ca0.5MnO3 and

CaMnO3, respectively) at two temperatures: 15 and 300

Kelvin (K).

All the K-edge SPXANES

spectra of La1-xCaxMnO3

are shown in Figure 1.

They reveal a marked

splitting between the spin

up and spin down channels of both the preedges (energy between

6.535 and 6.55 kiloelectronvolts (keV)) and

the main edges (energy

between 6.55 and 6.58

keV).

In Figure 2, we expand

Members of the team of scientists who performed the study

(from left to right): Trevor Tyson (lead author), Qing Qian,

and Chi-Chang Kao.
Science Highlights 2 - 34

Figure 1. SPXANES spectra of La1-xCaxMnO3 for x = 0,

0.3, 0.5, and 1. The solid and green lines correspond to

the spin up and down channel, respectively, measured

at 300 Kelvin.

Figure 3. Schematic diagram showing the transitions in the pre-edge for spin-polarized absorption of LaMnO3 in the lowtemperature A-type antiferromagnetically ordered state. (a) Local magnetic ordering of magnetic ions. (The oxygen atoms

are not shown for clarity.) (b) Allowed transitions for excitation of manganese, in which the d final state of a neighbor is of

the same spin polarization as the absorber (left panel) or the spin polarization is reversed (right panel).

Figure 2. Temperature-dependent pre-edge SPXANES

spectra of the region near feature a in Figure 1. The three

straight lines indicate the a1, a2, and a3 features.

Intensity(arb.units)

Energy(KeV) Energy(KeV) Intensity(arb.units)

the pre-edge region of the

SPXANES spectra. Three peaks (labeled a1, a2, and a3) in La1-

xCaxMnO3 (x = 0, 0.3, 0.5, and 1)

are observed. By examining the

changes in the pre-edge spectra for

temperatures above and below

magnetic ordering temperature, we

have developed an electron excitation model to understand the origin of the features a1, a2 and a3.

In Figure 3, we display our transition model, which shows that the

changes in the pre-edge region

with temperature can be directly

linked to changes in magnetic ordering of the manganese ions

around absorbing manganese sites.

The model also shows a transition

from a random local magnetic arrangement to an ordered arrangement.

Our model could be used to investigate a great range of perovskite

transition metal materials, and,

more generally, octahedrally-coordinated transition metal materials.

Our model and SPXANES measurements could also be used to predict magnetic ordering changes in

materials such as thin films, single

crystal or powders.
2 - 35 Condensed Matter Physics

FUNDING

Lucent Technologies

PUBLICATION

P. M. Voyles, D. A. Muller, J. L. Grazul, P. H.

Citrin, and H.-J. L. Gossmann, ìAtomicscale Imaging of Individual Dopant Atoms

and Clusters in Highly n-type Siî, Nature

416, 826 (2002).

FOR MORE INFORMATION

David Muller, Bell Laboratories, Lucent

Technologies, Murray Hill, New Jersey

davidm@bell-labs.com

BEAMLINE

X15B

The electrical properties of a semiconductor ñ a material having electrical conductivity greater than insulators but less than good conductors, and used especially as a

base material for computer chips

and other electronic devices ñ can

be controlled by adding small

amounts of foreign atoms, called

dopants. When dopants such as

antimony are added to a semiconductor such as silicon, the dopants

occupy lattice sites (the locations

occupied by atoms in the crystal)

in place of silicon atoms, and donate electrons, thus changing the

electrical properties

of the silicon.

The shrinking size of

electronic devices requires that the concentration of electrons ñ and therefore

the concentration of

dopants needed to

generate them ñ

must increase to

maintain device performance. However,

at the high dopant

concentrations

needed for future silicon device technology, not all the

Imaging Single Dopant Atoms and Clusters in

1

Bell Labs, Lucent Technologies, Murray Hill, NJ, 2Agere Technologies, Berkeley Heights, NJ

P. Voyles1, D. Muller1, J. Grazul1, P. Citrin1, and H. Gossmann2

Bulk Silicon

As silicon-based transistors in integrated circuits grow smaller, the concentration of charge carriers generated by impurity dopant atoms must

steadily increase to maintain the transistorsí performance. But current

technology is rapidly approaching the limit at which introducing additional dopant atoms ceases to generate additional charge carriers, because the dopants form electrically inactive clusters. Scientists from

Bell Laboratories have used x-ray absorption measurements at beam

line X15B of the National Synchrotron Light Source, and scanning transmission electron microscopy (STEM) to understand the nature of these

dopant clusters in silicon. The STEM data represent the first observation

of single atoms and clusters the size of a few billionths of a meter inside

a bulk solid, and they provide insight into how the clusters are formed.

dopants remain electrically active.

Instead, they form electrically inactive clusters. It is therefore important to understand how the

dopant atoms become electrically

inactive, leading to the observed

saturation of free-electron densities.

We have shown, by performing extended x-ray absorption fine structure (EXAFS) measurements at

beamline X15B that, in highly antimony-doped silicon samples,

the most commonly accepted models for the dopant clusters, in which

three or four antimony atoms surround a silicon vacancy, were not

correct. We used first-principles

calculations, which suggest that the

dominant clusters in these samples

contain only two dopant atoms with

no silicon vacancies.

These findings have now been

tested using scanning transmission

electron microscopy (STEM) on the

same antimony-doped samples after mechanically thinning them to

a thickness of less than five nanometers. (One nanometer is one billionth of a meter.) The thinning procedure was particularly demanding, because surface roughness and oxidation

had to be kept to a

minimum to ensure

maximum imaging

contrast between the

crystalline silicon and

antimony atoms. The

small sample thickness was important

for optimizing the likelihood that only a

single antimony atom

would occupy a given

column of silicon atoms when viewed in

projection.

Authors of the study (from left to right): David Muller, Paul Citrin

(seated), Hans Gossmann, John Grazul, and Paul Voyles (lead author).
Science Highlights 2 - 36

Figure 2. Calculated structures compared with

simulated and experimental scanning transmission

electron microscopy images of a donor-pair defect

cluster with 2 antimony dopant atoms and no siliconatom vacancy (left) and of a of 3-antimony-atom cluster

surrounding a vacancy (right). Antimony and silicon

atoms are in yellow and red, respectively. The silicon

atoms appear orange when in front of antimony atoms.

Figure 1. Scanning transmission electron microscopy image

of a cross-section of highly antimony-doped silicon. The

brightest dots (left) are atomic columns of one or more

antimony atoms, which are absent in the undoped sample

(right).

Figure 1 shows a STEM image of

a sample. The atomic columns of

silicon containing at least one antimony atom are seen as the brightest dots on the left, whereas no

such dots are seen in the undoped

region on the right. Applying filtering and particle-counting algorithms to such images from

samples only 2.3 and 1.5 nanometer-thick (corresponding to 11 and

9 silicon atoms per column) revealed that the distribution of single

dopant atoms was purely random.

This suggests that overcoming

free-electron density saturation at

very high dopant concentrations

will be a major challenge.

Figure 2 compares calculated

structures for clusters containing

two and three antimony atoms with

corresponding simulated and experimental images. Careful analysis shows that the two-atom clusters outnumber those with three or

four atoms by 50:1.

The observed random distribution

of dopants provides insight into the

formation mechanism of the clusters. We have recently performed

additional experiments and calculations to characterize the twoatom structures more completely,

and the results are being prepared

for publication.

Our study provides the first, unambiguous observation of single

dopant atoms within a bulk crystal. This observation paves the way

for further analysis of single atoms

and clusters of two to four atoms,

and for the study of the structure

of impurities and alloy constituents

in crystalline solids.
Geology and

Environmental Sciences
2 - 37 Geology and Environmental Sciences

Scientists have provided new evidence for the existence of iron sulfide ñ iron combined with sulfur ñ

in comets, which are large chunks

of ice and rock that have remained

nearly unchanged since the beginning of the solar system. The catalytic behavior of iron sulfides is

involved in the formation of hydrocarbons ñ key building blocks of life

ñ so this discovery reinforces the

idea that seeds of life may have

come to Earth from comets. The

results of the study are described

in the May 9, 2002 issue of Nature.

ìSulfur is one of the more abundant elements in space,î says Lindsay Keller, a scientist at NASAís

Johnson Space Center (JSC) and

lead author of the study, ìyet astronomers have never been able to

account for it around young stars

ñ until now.î

Two groups of scientists participated in the study. The first looked

at dust particles coming from comets and falling in Earthís atmosphere. The second made astronomical observations of the disks

of dust and gas surrounding young

stars, and determined the chemical composition of these disks.

ìWhen the solar system formed,

the dust that was not swept up in

the solar system ended up in comets,î Keller says. ìThis dust has

been sitting inside the icy comets

for 4.5 billion years. So comets represent a sort of a freezer of presolar materials. By looking at the

particles given off by comets, we

can track down the particles that

were present in the beginning of

the solar system.

ìAnother way to understand how

our solar system started to form is

to look at disks of dust and gas

Scientists Provide Evidence that Life on Earth May Have

Come from Comets

around young stars,î he adds.

ìWhat happens there is very similar to what is thought to have occurred in our solar system.î

Cosmic vs. Earth Dust

Although the origin of comets is still

uncertain, scientists believe that

most reside outside the orbits of

the planets in the Kuiper belt and

Oort cloud. As a comet makes its

way towards the sun, it releases

dust and gases as the surface is

warmed. A fraction of the dust that

is released is swept up by the Earth.

ìBecause these particles are so

small, many of them slow down in

the upper atmosphere (at ~100 km

altitude) without getting strongly

heated ñ so they are not strongly

altered ñ and they slowly settle

over weeks to months on to the

ground,î Keller says, adding that

the Earth accretes roughly 40,000

tons of interplanetary dust each

year.

NASA has, for the past two decades, sent aircraft with special

sticky collectors to altitudes of 12

to 14 miles to capture the cosmic

dust as it falls through the stratosphere before it becomes mixed

with Earth dust.

The collected dust particles, which

are one-tenth the diameter of a

human hair, are examined in the

ultra-clean Cosmic Dust Laboratory

at JSC.

ìThe dust particles are so tiny that

they are invisible to the naked eye,î

Keller says, ìso you need a microscope to see them and a very clean

environment not to contaminate

them with dust coming from the

air.î

Scientists wearing clean-room

overalls ñ often called ìbunny suitsî

ñ use high-resolution, light optical

microscopes to examine the morphological characteristics and

chemical composition of the parThe inner solar system is suffused with a vast cloud of interplanetary dust. This

dust cloud is invisible to the naked eye as the zodiacal light - a triangular glow

rising above the horizon shortly after sunset or before sunrise. The picture to the

right shows the zodiacal light together with comet Hale-Bopp. (Courtesy of Richard

Wainscoat).
Feature Articles 2 - 38

ticles carefully. The particles are

then stored in dust-free, nitrogenfilled cabinets, which are available

to other scientists for more detailed

investigations.

Ultra-thin samples of dust

But the dust particles are so tiny

that scientists cannot handle them

easily. To investigate the chemical

composition of some of the dust

particles, Keller and his colleagues

John Bradley, George Flynn and

Don Brownlee surround the particles by beads of epoxy resin 10

to 20 times larger than the grains,

thus making the beads easier to

handle than the grains. ìHaving a

dust grain inside an epoxy bead is

like having a bug inside of an ice

cube,î Keller says.

Once the epoxy hardens, the scientists mount the bead on a

sample-holding device called a microtome, which is a very finelymachined instrument that cuts the

bead into extremely thin slices, the

thickness of each slice being three

thousandth of the beadís diameter.

ìIron sulfide is a very dense and

strongly absorbing mineral,î Keller

says, ìso when the samples are

that thin, you can finally get light

through the sample.î

The scientists determined the composition of the dust-containing slice

by using two complementary techniques. The sample was first analyzed at JSC with a transmission

electron microscope, in which electrons are sent through the sample

to reveal its atomic structure and

chemical composition. The slice of

dust was also studied by using very

intense light from beamlines U10B

and X1A at the NSLS. By looking

at how infrared light is absorbed in

the samples, the scientists can determine what kinds of minerals and

compounds are present in the particles.

Keller and his colleagues discovered

that several of the dust particles

were mainly made of iron sulfides.

ìWhen we looked at the infrared

spectra, lo and behold, we had a

very nice signal that corresponded

exactly to iron sulfide,î Keller says.

Using very intense light was key to

the detection of iron sulfide, he

adds, because the samples are ìso

small and so thinî that the intensity generated by the sample is too

weak to be detected by off-theshelf lab instruments. ìThe infrared intensity in NSLSís VUV ring is

about 500 ñ 1000 times brighter

than conventional instruments,

which translates into a much improved signal,î he says.

But more exciting results awaited

Keller and his colleagues when they

compared their results with those

of another group of scientists looking at young stars trillions of miles

away from Earth.

An unknown signal from

the cosmos

What inspired Keller and his collaborators to analyze their particles

were the results from astronomers

studying the chemical composition

of disks of dust and gas around two

stars recently formed. The two balls

of fire, called the Herbig stars, are

surrounded by disks of dust and

gas, which have not given birth to

planets yet ñ if planets were to

arise from the disks.

The scientists studied the two stars

with the Infrared Space Observatory Observatory (ISO), an astronomical satellite that investigated

the infrared light emitted by the

dust and gas surrounding fledgling

stars from 1995 to 1998.

The scientists, working at the Astronomical Institute in Amsterdam

in The Netherlands, the European

Space Agency in Noordwijk, The

Netherlands, and the Astronomical

Institute and University Observatory in Jena, Germany, identified

many of the chemical elements

present in the two stars. But, when

they decided to remove from the

starsí infrared spectra the contributions from all known elements,

a signal of unknown origin appeared.

ìWhen the astronomers subtracted

everything from their spectra that

they knew was there ñ the silicates, Cosmic Dust Laboratory (CDL) at NASA JSC.
2 - 39 Geology and Environmental Sciences

the glasses, the carbon, and ices ñ

there was always a big residual feature,î Keller says.

Iron sulfide revealed again

ìThe ISO scientists interpreted the

signal incorrectly as being possibly due to iron oxide,î Keller says.

ìIn fact, our signal occurred at the

same position on the spectra as

their signal. It was a very nice

match in terms of peak position,

shape, and width.î

After studying carefully their spectra, the two groups agreed that the

ìunknownî signal was indeed produced by iron sulfide. They also

considered spectra of terrestrial

samples known to contain iron sulfide and found that they also

matched very well with their respective experimental spectra.

The researchers also found that

their results agreed with predictions on the abundance of solid

sulfur around young stars. ìAstronomers have predicted that sulfur was all present as dust grains,

not in the form of gas,î Keller says.

ìOur results could account for the

abundance of sulfur in the iron sulfide grains, as predicted.î

Seeds of life?

By showing for the first time that

iron sulfides are both present in

comets and around young stars,

Keller and his collaborators provide

further evidence that ìseeds of life,î

in the form of dust grains or hydrocarbon molecules, may have led

to the development of life on Earth.

ìMany of the current models for

how Earth acquired early organic

molecules are from particles that

came out of space,î Keller says. ìSo

comets may have brought to Earth

the chemicals that are necessary

to life, such as organic molecules

and water.î

The first two spectra are from terrestrial standards, which are samples known to

contain iron sulfide. The two spectra in the middle are from observations of

young stars called the Herbig stars. In these spectra, the scientists have subtracted

all the known components such as silicates, ices, and carbon from the original

spectra. The bottom two spectra are from dust particles, found to be very rich in

iron sulfide. All three types of spectra show a peak that is infrared active at the

same wavelength. Keller and his collaborators show that the peak is due to iron

sulfide, a chemical that was probably present during the early times of the solar

system formation and may have sowed the seeds of life on Earth.

It is interesting to consider that

ìseeds of lightî may have been

pouring on Earth from the sky since

Earthís creation. ìI am fascinated

to be working on grains of materials that are older than the solar

system, ìKeller says. ìTo realize

that the accumulation of vast

amounts of star dust that ended

up forming our sun and the planets around it is just as fascinating.î

BEAMLINE

U10B and X1A

PUBLICATION

L.P. Keller, et al., ìIdentification of

Iron Sulphide Grains in

Protoplanetary Disks,î Nature,

417, 148 (2002).

 -Patrice Pages
Feature Articles 2 - 40

Recent research at the NSLS, reported in the October 24, 2002 issue of Nature by Stony Brook University (SBU) scientists, illustrates

for the first time why earthquakes

do not start in the Earthís lower

mantle, the lower part of the

roughly 1,400-mile-thick portion

surrounding Earthís core.

Using bright, hard x-rays from the

superconductor wiggler beamline

X17, Jiuhua Chen of SBUís Mineral

Physics Institute led research in

measuring the strength of Mg 0.9

Fe 0.1 SiO3 perovskite, a dominant

mineral of the lower mantle, at high

pressure and temperature. Collaborators in this research, which

is funded by the National Science

Foundation, are Donald Weidner

and Michael Vaughan, both of SBU.

ìWe found that the perovskite not

only is stronger than other minerals at high pressure and temperature, but also has a temperatureinsensitive plastic-flow character,î

said Chen. ìThe result revises the

existing prediction of the rheological property ó which is the flow of

a material under stress ó of Earthís

lower mantle and thus supplies the

first experimental evidence for understanding why earthquakes do

not start in the lower mantle.

ìThis result also sheds light on

many other of Earthís dynamics,î

added Chen.

He explained that, from surface to

center, Earthís structure is made up

of the crust; the upper mantle; the

transition zone; the lower mantle;

the outer core, which is liquid; and

the inner core. Earthís crust is divided into areas called tectonic

plates which move separately and

rub against each other. Some

earthquakes occur when adjacent

plates ìcatchî and then suddenly

release the pressure that has built

up over time. These are called

near-surface or shallow earthquakes.

When two plates collide, the thinner, denser plate is forced under

the thicker, lighter plate and sinks

deep into the mantle. This process

is called subduction.

Earthquakes can also start along

the subducting slab. These earthquakes are called deep earthquakes.

SBU Researchers at the NSLS Discover Properties of Perovskite,

Explain Why No Earthquakes Start in Earthís Lower Mantle

Jiuhua Chen is at beamline X17B at the NSLS, where a Stony Brook University team has developed equipment that can

simulate temperature and pressure conditions needed for studying Earthís structure and dynamics.
2 - 41 Geology and Environmental Sciences

ìOur result helps in understanding

more about the deflection of the

subducting slab at the top of the

lower mantle, because the strong

perovskite may create a mechanical barrier to the subduction,î said

Chen. ìWe can now also predict a

viscosity jump at the boundary

between the transition zone ó the

portion of Earth that is between

250 and 410 miles deep ó and the

lower mantle, which is very important information for modeling convection processes in Earth.î

Chen explained that the mechanism of deep earthquakes has been

a long-standing question. Geophysicists know that seismic observations show no earthquakes starting in the lower mantle, but until

the SBU study of perovskite, the

reason was unclear.

ìWe have studied the rheological

properties of many mantle minerals,î Chen said. ìOur results indicate that, among many possible

mechanisms, plastic instability may

be responsible for the earthquakes.î

Investigating the properties of

perovskite is difficult because this

mineral, unlike others, is unstable

under ambient conditions.

ìHowever, with the experimental

instrumentation that we developed

at the NSLS, we could finally challenge the problem,î said Chen. ìOur

goal is to gain a full understanding

of Earthís structure and dynamics.

With the NSLS right on our doorstep, we are approaching this goal.î

-Liz Seubert

[Editorís note: Reprinted with permission from the BNL Bulletin - November

1, 2002.]
2 - 43 Geology and Environmental Sciences

FUNDING

Lawrence Livermore National Laboratory,

Department of Energy (DOE)

PUBLICATION

H. Cynn, J. E. Klepeis, C.-S. Yoo, and D. A.

Young, "Osmium has the Lowest

Experimentally Determined Compressibility," Physical Review Letters 88, 135701

(2002).

FOR MORE INFORMATION

Hyunchae Cynn, High-Pressure Physics

Group, Lawrence Livermore National

Laboratory, Livermore, California

cynn1@popeye.llnl.gov

BEAMLINE

X17C

Osmium Is Stiffer Than Diamond

H. Cynn1, J.E. Klepeis1, C.-S.Yoo1, D.A. Young1

1

Lawrence Livermore National Laboratory, University of California, Livermore, California

Scientists from the U.S. Department of Energyís Lawrence Livermore

National Laboratory (LLNL) working at the NSLS and LLNLís Stanford

Synchrotron Radiation Laboratory have reported the surprising discovery that metallic osmium is stiffer than covalently bonded diamond. The

researchers also found that iridium and ruthenium are as incompressible as rhenium. In addition, they performed first-principles calculations

that independently confirm the observed trend in the transition metal

bulk moduli.

Diamond is the hardest known

material. However, in searching for

other hard materials it is generally

simpler to study the compressibility, which is often correlated with

the hardness. The compressibility

is a measure of how much the volume changes for a given change in

pressure and is equal to the reciprocal of the bulk modulus. A material that has a low compressibility

(incompressible, high bulk modulus) is stiff or difficult to compress.

In addition to being the hardest

known material, diamond also

held the record for the highest bulk

modulus at 443 gigapascals (4.43

million times atmospheric pressure). However, our newly measured value of 462 gigapascals for

osmium exceeds that of diamond.

We also found that iridium and ruthenium are as incompressible as rhenium,

which has previously been

reported to be a strong

metal.

It has long been known on

the basis of the simple

Friedel model of chemical

bonding in transition metals that the largest bulk

moduli should occur in the

middle of each transition

metal row in the periodic

table. The position of osmium in the middle of the 5d row

is thus consistent with the high

value of the bulk modulus we have

obtained. As far as we know, no

compressibility data for osmium at

high pressures have been reported

previously.

We performed compression studies with a diamond-anvil cell (Figure 1) up to 65 gigapascals for osmium, ruthenium, and iridium.

Condensed argon was used as a

pressure medium, and ruby grains

smaller than three micrometers in

diameter were used to determine

the pressure. Powder samples with

grain sizes less than five micromeMembers of the LLNL high-pressure physics experimental group and

collaborating theoretical physicists. Physicist Hyunchae Cynn (front), who is

the lead author of the study, is holding a diamond-anvil cell of the type used

in the osmium experiments.

Figure 1. Two opposing diamond anvils

supported by tungsten carbide mounts provide

a sample chamber by placing a metal gasket in

between the flat tips (approximately 300

micrometers in diameter) of the two diamond

anvils. The gasket has a small hole (less than

100 micrometers) drilled at the center.
Science Highlights 2 - 44

Figure 2. Energy-dispersive x-ray diffraction pattern (EDX)

of osmium at 65 gigapascals. Inset shows expanded view

from 70 to 80 keV. The EDX were measured at the X17C

beamline of NSLS, using unfocused white x-rays from the

superconducting wiggler beam.

Figure 3. Volume compression data for osmium,

fit with the Birch-Murnaghan equation of state,

yielding the bulk modulus B0 and its first pressure

derivative of B0

í

.

Energy (keV)

Intensity (a.u.)

P(GPa)

V/V0

ters were contained inside a small

hole (80 micrometers in diameter)

drilled into a rhenium gasket.

The measured diffraction patterns

were dispersed either in energy

using unfocused white x-rays from

the superconducting wiggler

beamline X17C at NSLS, or in angle

using focused monochromatic xrays from the wiggler beamline 10-

2 at SSRL. Figure 2 shows a typical energy-dispersive x-ray diffraction pattern for osmium at 65

gigapascals, consisting of the diffraction lines from hexagonal close

packed osmium and face-centered

cubic argon, and the x-ray emission lines from osmium.

Measured compression data for

osmium, iridium, and ruthenium

were fit using the third-order BirchMurnaghan equation of state

(EOS). The osmium data and fit are

both shown in Figure 3. We have

also carried out first-principles calculations of the EOS for these three

metals. The calculations yield the

same trend in the bulk moduli, thus

providing an independent confirmation of our experimental results.

In summary, we found that osmium

has the largest bulk modulus yet

measured. This result provides impetus for a continued search for superhard materials, including transition metal carbides, nitrides,

borides, and oxides.
2 - 45 Geology and Environmental Sciences

FUNDING

US National Science Foundation,

North Carolina Agricultural Research

Service (NC-ARS)

PUBLICATION

S. Beauchemin, D. Hesterberg, and M.

Beauchemin, ìPrincipal Component

Analysis Approach for Modeling Sulfur KXANES Spectra of Humic Acids,î Soil Sci.

Soc. Am. J., 66, 83-91(2002).

FOR MORE INFORMATION

Suzanne Beauchemin, Research Scientist,

Soil and Water Chemistry, Natural

Resources Canada, Environmental Lab.,

Ottawa, Ontario, Canada

sbeauche@NRCan.gc.ca

BEAMLINE

X19A

X-ray absorption near edge structure (XANES) spectra from unknown soil samples are usually

modeled using techniques called

spectral deconvolution and/or

least-squares linear combination

fitting (LCF). Both approaches rely

on a priori information. Spectral

deconvolution is based on an assumption about the shape of the

band, while least-squares LCF involves fitting pure standard species

to resolve an unknown

mixture.

We tested a different

modeling technique,

called principal component analysis (PCA), to

analyze soil mixtures.

This technique considers

the statistical variance

within an experimental

data set composed of a

group of unknown

samples. The data set is

first redefined in terms

of a reduced number of

independent sources of

variability, called components. These components have no chemical

or physical meaning.

A subsequent analysis,

Characterization of the chemical species of trace elements in soils, sediments, and other geochemical systems is essential for predicting their

solubility and potential mobility in the environment. To determine metal

speciation, scientists usually model x-ray absorption near edge structure (XANES) spectra by using standards of well-defined chemical species. But when scientists deal with complex matrices such as soilñ in

which many different chemical forms of the element may co-exist ñ

other modeling techniques called principal component analysis (PCA)

and target analysis, might be more convenient to use. The PCA was

successfully applied to sulfur K-XANES spectra of six humic acid samples.

Modeling Sulfur K-XANES Spectra of Humic

Acids With the Principal Component Analysis

Approach

the target transformation, is used

to test if suspected known species

are part of the structural variation

of the sample set. Based on the

results from target analysis, abstract matrices obtained in the first

step are transformed into chemically meaningful matrices.

A major advantage of the PCA approach is that no a priori assumption is needed regarding the shape

of the band. Also, suspected species can be evaluated individually

without a priori knowledge of other

species present in the sample.

PCA coupled with target transformation was used to model sulfur

K-XANES spectra of six soil humic

acid samples (Figure 1) using the

spectra of seven chemical compounds as sulfur standards: sodium

sulfate, chitin sulfate, cysteic acid,

benzyl sulfoxide, benzyl disulfide, elemental

sulfur, and methionine.

The objective was to

compare the results

from PCA approach to

those obtained from

least-squares LCF.

PCA identified three

main components. As

illustrated in Figure 2,

target analysis showed

how closely the predicted targets fitted the

suspected known species. Chitin sulfate was

a better sulfate species

than sodium sulfate to

explain our experimental data. Sodium sulfate, cysteic acid and

benzyl disulfide were

S. Beauchemin1, D. Hesterberg2, and M. Beauchemin1

1

Natural Resources Canada, Ontario, Canada; 2North Carolina State University, Raleigh

(Authors from top,

clockwise): S. Beauchemin,

D. Hesterberg, and M.

Beauchemin
Science Highlights 2 - 46

Figure 2. Predicted targets obtained through target transformation of the sulfur K-XANES spectra for (A) sodium sulfate,

(B) cysteic acid, (C) benzyl disulfide, and (D) chitin sulfate compared with the normalized K-XANES spectra for these

species. The energy scale is relative to S(0) K-edge at 2472 eV.

Figure 1. Soil humic acids were extracted from

a coastal salt marsh in eastern North Carolina.

Soils in salt marshes such as this one near

Beaufort, NC, contain reduced organic sulfide

that has a high binding affinity for mercury and

perhaps other trace elements. (Photo courtesy

of Stephen W. Broome, NC State.)

marginal candidates, which means

that the nature of the real species

in the spectra of humic acids may

be slightly different. Other standards were rejected. Therefore, we

retained chitin sulfate, cysteic acid,

and benzyl disulfide to derive the

relative proportion of each selected

standard species in each sample.

The PCA approach provides a statistical basis for (i) gaining insight

into the identification of chemical

species in a multi-component

sample, and (ii) defining the number of individual species to include

in the spectral fitting. Therefore, it

is a valuable complementary tool

for band resolution or LCF as it

helps to avoid an excessive number of bands or standards in the

fit.
2 - 47 Geology and Environmental Sciences

PUBLICATION

K.G. Scheckel and J.A. Ryan, ìEffects of

Aging and pH on Dissolution Kinetics and

Stability of Chloropyromorphite,î Environ.

Sci. Technol. 36, 2198 ñ2204 (2002).

FOR MORE INFORMATION

Kirk Scheckel, U.S. Environmental

Protection Agency, Office of Research and

Development, National Risk Management

Research Laboratory, Land Remediation

and Pollution Control Division,

Remediation and Containment Branch,

Cincinnati, Ohio

Scheckel.Kirk@epa.gov

BEAMLINE

X11A

Previous research has shown that

adding phosphate materials to

lead-contaminated soils leads to an

environmentally stable and biologically inert lead mineral called

chloropyromorphite (Pb5(PO4)3Cl).

Because chloropyromorphite is the

most stable lead mineral known,

other solid-phase lead species

should be transformed to

chloropyromorphite by a dissolution-precipitation mechanism to

immobilize soluble soil lead in situ

by simply adding phosphate to the

soil. But the long-term fate of immobilized lead as precipitated

chloropyromorphite is not fully understood.

We investigated the kinetics of dissolution and crystallization dynamics of synthetic chloropyromorphites with increasing aging

times ranging from one hour to one

year, to understand better what

may be happening in the field setting. The chloropyromorphites

were dissolved in a solution containing not only phosphoric acid,

but also nitric acid, thus simulating environmental conditions one

may find in areas ranging from acid

mine drainage to agricultural soil

settings.

Influence of Aging and pH on Dissolution

Kinetics and Stability of Pyromorphite

Immobilization of metal contaminants in soil shows great potential as a

cost-effective and environmentally friendly remediation technique. Leadcontaminated soils are typically removed from site and replaced with

clean soil at great costs. Innovative technologies for sequestering lead

in situ have been proposed and studied. One of these methods, called

immobilization-remediation, seeks to both sequester most of the contaminant and retain the metal for the long-term. Scientists at the Environmental Protection Agencyís Office of Research and Development in

Cincinnati, Ohio, have examined how the most stable lead mineral, called

chloropyromorphite, forms and dissolves over time, thus providing a

better understanding of lead sequestration in soil.

The objectives of this research were

to understand the effect of aging

time on the stability of

chloropyromorphite dissolved in

phosphoric and nitric acid, to examine physical and chemical alterations of the chloropyromorphite

samples, and to model the kinetic

data collected from the dissolution

experiments. Aging of the samples

prior to dissolution was investigated by using x-ray absorption

fine structure (XAFS) and x-ray diffraction (XRD) spectroscopies, and

the stability of the chloropyromorphite material with temperature was studied with high-resolution thermogravimetric analysis

(HRGTA).

Figure 1 shows data for XAFS,

XRD, and HRTGA analyses of aged

chloropyromorphite prior to dissolution. The XAFS data (Figure 1a,

solid line), collected at beamline

X11A of the National Synchrotron

Light Source (NSLS), show relatively little difference between the

one-hour and one-year samples.

These same chloropyromorphite

samples were also examined by

XRD (Figure 1b) and, again, do

not suggest any alteration in the

chemistry or crystallinity of the

chloropyromorphite phases as aging time increases. But HRTGA

showed that aging of the

chloropyromorphite crystals did

change with increasing residence

time (Figure 1c), suggesting, perhaps, an increase in the crystalsí

Ostwald ripening, in which small

crystals, more soluble than large

ones, dissolve and re-precipitate

onto larger particles.

The dissolution experiments conducted for this research were designed to observe and compare

data as influenced by aging time,

pH (potential Hydrogen) of the dissolution agent (the pH describes

the hydrogen-ion activity of the

solution, and determines if the soK.G. Scheckel and J.A. Ryan

U. S. Environmental Protection Agency, Office of Research and Development, National Risk

Management Research Laboratory, Cincinnati, Ohio

Kirk Scheckel
Science Highlights 2 - 48

Figure 1. (a) X-ray absorption fine

structure (XAFS) spectroscopy, (b) Xray diffraction (XRD) spectroscopy,

and (c) high-resolution thermogravimetric analysis (HRGTA) of aged

pyromorphite samples.

lution is acid, basic or neutral), and

dissolution method (stirred flow or

mixing in batches, instead of continuously, also called batch

method).

Regardless of pH or dissolution

method, it appeared that the onehour-aged chloropyromorphite was

the most soluble. Aging of

chloropyromorphite from one day

to one year did not lead to a significant increase in stability, suggesting that crystal aging was accomplished within 24 hours.

We also observed that, as the pH

of the nitric acid decreased, the

amount of released lead increased.

By removing the dissolution reaction products in the stirred-flow

experiments, more chloropyromorphite was dissolved in the

stirred-flow than in the batch studies, the difference in released lead

between these two methods becoming more pronounced as pH

increased. So, once chloropyromorphite forms in contaminated

soils and sediments, it should remain immobilized and stable in

these environments under nearneutral pH.

The potential impact of stabilization remediation methods to safely

sequester metal contaminants in

the natural environment holds

great promise but must be managed carefully and intelligently. The

results of this work and of others

demonstrate that chloropyromorphite formation can be easily

accomplished by the reaction of

available lead and phosphorus. Our

study suggests that chloropyromorphiteís persistence would endure most environmental conditions, thus making lead-immobilization via phosphorus an ideal

remediation mechanism.

Figure 2. Crystals of chloropyromorphite.
2 - 49 Geology and Environmental Sciences

FUNDING

Swiss Ministry of Science and Education

PUBLICATION

A. Voegelin et al., ìSlow Formation and

Dissolution of Zn Precipitates in soil: A

Combined Column-transport and XAFS

Studyî, Environ. Sci. Technol. 36, 3749

(2002).

FOR MORE INFORMATION

Ruben Kretzschmar, Soil Chemistry

Group, Institute of Terrestrial Ecology,

Swiss Federal Institute of Technology,

Zurich, Switzerland

kretzschmar@ito.umnw.ethz.ch

BEAMLINE

X11A Slow Precipitation and Dissolution of Solids

Affects the Mobility of Heavy Metals in Soils

What happens if soils are contaminated with heavy metals by agriculture, mining, or industry? Will the metals slowly leach into groundwater

and pollute our drinking water resources? Will they be taken up by plants

and finally end up in our diet? Environmental soil chemists are trying to

answer these questions by determining the chemical forms, or species,

of heavy metals in soils. Scientists at the Swiss Federal Institute of

Technology in Zurich, Switzerland, have combined x-ray absorption finestructure (XAFS) spectroscopy with a chromatographic soil column technique to determine the species and mobility of heavy metals in a typical, slightly acidic soil. Their results suggest that some metals (such as

zinc) were relatively tightly bound by forming mineral precipitates, while

others (such as cadmium) remain highly mobile.

Soil, or ìdirt,î as some people call

it, is made up of an extremely complex mixture of minerals and natural organic substances. So, trying

to understand how contaminants

behave in such a complex environment might seem daunting, but soil

chemists are currently making

rapid progress by combining field

observations and controlled laboratory experiments with modern

spectroscopic techniques.

Our research team has combined

two techniques, a chromatographic

soil column technique and X-ray

absorption fine structure spectroscopy (XAFS) to investigate the chemical

behavior of zinc and

other transition metals in a slightly acidic

loamy soil, at realistically low metal concentrations.

Previous experiments

have suggested that

certain transition

metals including cobalt, nickel and zinc

can form structures

called layered double

hydroxide (LDH)

when these metals

chemically react with clay minerals in neutral soils (neither acidic,

nor basic) and relatively high metal

concentrations. But these experiments have not shown clearly

whether such structures can form

in soils under more acidic conditions and at realistically low concentrations of metals from an infiltrating solution.

The objectives of our study were:

(1) to investigate the rapid and

slow absorption of cobalt, nickel,

zinc and cadmium in a slightly

acidic loamy soil; (2) to examine

the subsequent release of metals

due to cation exchange and soil

acidification; and (3) to assess the

predominant absorption mechanisms of zinc in the soil.

One of the key techniques that we

used is a chromatographic soil column technique. The basic idea is

to pack a column with soil, and then

leach it over a long time period with

a solution containing small concentrations of cobalt, nickel, zinc and

cadmium. When solid precipitates

form slowly, the products accumulate over time in the soil column.

At the end of this loading period,

we can identify the precipitates and

study how they redissolve by following changes in solution chemistry.

Solid precipitates of

zinc were identified

by using a technique called x-ray

absorption finestructure (XAFS)

spectroscopy at

beamline X11A of

the National Synchrotron Light

Source. In this technique, x-rays generated at the NSLS

A. Voegelin, A.C. Scheinost, K. B ̧hlmann, K. Barmettler, and R. Kretzschmar

Soil Chemistry Group, Institute of Terrestrial Ecology, Swiss Federal Institute of Technology,

Zurich, Switzerland

Some of the Authors of the study (from left to right): Andreas C.

Scheinost, Andreas Voegelin (lead author), Kurt Barmettler, and Ruben

Kretzschmar.
Science Highlights 2 - 50

Figure 1. Identification of zinc species with x-ray absorption fine structure (XAFS) spectroscopy. After a slightly acidic soil

column has reacted with a dilute zinc solution, zinc atoms are coordinated to six oxygen atoms at a distance of 2.07

angstroms (one angstrom is one tenth of a billionth of a meter), and to three or four zinc atoms at 3.10 angstroms. This

local structure (middle curve) is similar to the solid phase zinc-aluminum-layered double hydroxide (Zn-Al-LDH), but is

unlike the zinc inner-sphere surface complex. The structural drawings on the right side depict the two binding mechanisms

(green: zinc octahedral; gray: aluminum octahedral; red: silicon tetrahedral; yellow: aqueous cations).

are projected toward the precipitate, in which some of the photons

of light are absorbed. By measuring the ratio of absorbed photons

versus the total incident photons

as a function of the energy of the

incident photons, we can determine

the nature of the chemical elements present in the precipitate.

Figure 1 shows three spectra,

called radial structure functions,

obtained by applying the XAFS

technique to zinc-aluminum-LDH

synthesized in the laboratory, soil

from the column experiment after

41 days of loading, and the same

soil with zinc adsorbed in a geometry called inner-sphere surface

complex (Figure 1, bottom right).

By analyzing the spectra, we suggest that a solid phase similar to

zinc-aluminum-LDH has formed in

the soil column. While zinc-aluminum-LDH and zinc-phyllosilicate (a

phyllosilicate is a type of silicate

mineral) cannot be distinguished

easily based on the local structure,

our leaching experiments demonstrate that the precipitates formed

in the soil are readily re-dissolved

upon acidification. Because zincphyllosilicates are expected to be

much less soluble, formation of

zinc-aluminum-LDH seems most

likely.

When different transition metals

were compared, we found that the

importance of precipitation of solid

phases in the slightly acidic soil

decreased in the order zinc-nickelcobalt-cadmium, where zinc is the

most tightly bound and cadmium

is the most mobile. Our study has

demonstrated that combining wellcontrolled laboratory studies with

XAFS spectroscopy is a promising

approach to investigate the behavior of metal contaminants in soils.
Life Sciences
2 - 51 Life Sciences

Funded by DOE and the National

Institutes of Health, three new enzyme studies at BNL have yielded

a new strategy for blocking infection by human adenovirus. The

findings, reported in the October,

November, and December, 2001 issues of the journal, Biochemistry,

have already been used to design

novel antiviral drugs.

Adenoviruses cause a number of

acute infections, including respiratory and gastrointestinal infections,

and conjunctivitis. In patients with

compromised immune systems,

such as those infected with human

immunodeficiency virus (HIV), an

opportunistic adenovirus infection,

is frequently deadly.

ìOur new antiviral drugs are expected not only to inhibit adenovirus, but also, possibly, to be effective against other organisms that

use the same enzyme - including

Chlamydia, one of the most prevalent sexually transmitted bacteria,

and Yersinia pestis, the organism

that causes the black plague,î said

Walter Mangel, Biology Department, the lead scientist on the

studies.

Infection Process

During infection, these viruses

make an enzyme called a protease,

which cleaves or degrades other

proteins. The protease is used by

the virus to complete the maturation of newly synthesized virus particles.

To explain this process, Mangel

uses the example of building a cathedral around internal scaffolding.

Once the cathedral is in place, the

last step is to remove the scaffolding. ìSimilarly,î says Mangel, ìadenovirus particles are built with

scaffolding proteins inside. Once

Enzyme Studies May Lead to New Antiviral Agents

the virus particle is formed, the

protease becomes activated and

cleaves the scaffolding to render

the virus particle infectious.î

The three recent studies at BNL

reveal that the protease is initially

synthesized in an inactive form.

The inactive enzyme binds to the

viral DNA to become partially activated.

The partially activated enzyme then

cleaves out a cofactor, which is a

protein fragment that binds to the

protease to activate it further. The

fully active complex of enzyme and

cofactor then moves along the viral DNA, cleaving the scaffolding

proteins.

ìSuch activation of a protease by

DNA has never been seen before,î

Mangel said. And this presented a

problem.

ìTwo other laboratories repeatedly

claimed in the literature that they

saw no stimulation of the enzyme

by DNA,î Mangel continued. ìSo,

in one of the three papers, we not

only presented definitive evidence

that the enzyme interacted with

DNA, but also showed why the two

other groups had not seen stimulation of the enzyme by DNA. Essentially, they did not use the correct conditions. We hope that, with

the publication of these papers, this

controversy is now resolved.î

Walter Mangel
Feature Articles 2 - 52

Next Step: To Design

Drugs

ìThese studies suggest that drugs

that bind to the active site of the

enzyme, which is the part involved

in cleaving proteins, the cofactor

binding site, or the DNA binding site

should block the enzymeís action

and serve as effective antiviral

agents,î Mangel said.

To design drugs able to bind to and

block these sites, the scientists first

had to characterize the molecular

structures. The active site of the

enzyme had been previously characterized by William McGrath, a

postdoc in Mangelís team, using an

intense beam of x-rays available at

the NSLS. The pattern of x-rays

bouncing off the atoms reveals the

three-dimensional molecular structure.

In the current studies, Stony Brook

University graduate student Mary

Lynn Baniecki characterized the

binding of the cofactor to the protease, identifying which parts bind

to the enzyme and which parts

stimulate the enzymeís activity.

McGrath and Baniecki then deciphered how the protease binds to

the DNA.

Among the other coauthors of the

study, Mangel said, are three undergraduate students, David

Green, Caroline Li, and Sarah

McWhirter, who were participants

in the DOE Energy Research Undergraduate Laboratory Fellowships program managed at BNL by

the Office of Educational Programs.

New, Three-Pronged

Therapy

Based on the findings, Mangel has

proposed a new form of antiviral

therapy using three different drugs

against these three target sites -

the active site, the cofactor binding site, and the DNA binding site -

on the same virus-coded protein.

This three-pronged approach may

overcome one of the biggest challenges in antiviral therapy - the

spontaneous evolution of drug-resistant strains.

As Mangel explains the idea, a

mutation conferring drug resistance at one site may alter the

physiological functions at the other

two sites because the three sites

are interdependent, thereby making drug resistance much less likely

to arise.

ìThe adenovirus protease may be

a good model system within which

to test the efficacy of this form of

combination therapy,î Mangel said.

Already, his team has developed

two new drugs, one that binds reversibly and another irreversibly to

the active site of the protease.

These drugs will soon be tested as

antiviral agents by the National

Institutes of Health.

A graphic representation of the structure of the

adenovirus protease. The active site is in the groove at

the top where the ìball-and-stickî figures are located.

The cofactor is the strand in the center at the bottom.

The DNA binding sites are identified with ìplus (+)î

signs.

- Karen McNulty Walsh

[Editorís note: Reprinted with permission from the BNL Bulletin - January

18, 2002.]
2 - 53 Life Sciences

Anti-Alzheimerís Drug Mechanism Revealed With X-Rays

Using x-rays produced by the

NSLS, a team of scientists has

gained new insight into the effects

of a newly approved drug, called

rivastigmine, in the treatment of

Alzheimerís disease ñ a debilitating brain disease causing memory

loss and other cognitive deficits in

about 10 percent of the elderly. The

new results, which may provide important information for generating

improved drugs for this as-yet incurable neurodegenerative disease,

were published in the March 19,

2002 issue of the American Chemical Society journal Biochemistry.

ìWe were very surprised by our results,î says Joel Sussman, a structural biologist at the Weizmann Institute of Science in Rehovot, Israel, and the lead author of the

study. ìThey show that we can

safely treat Alzheimerís disease

with much lower quantities of

rivastigmine, thus minimizing unwanted adverse effects.î

Though the drug is currently available under the trade name Exelon,

its mechanism of action at the

atomic level had not been studied

until now. So, the team of scientists, composed of Sussmanís team

and scientists from Novartis, a

pharmaceutical company based in

Basel, Switzerland, decided to take

a close look at how the drug helps

to slow the memory loss of

Alzheimerís patients.

One of the main pathological phenomena in Alzheimerís disease is

the deterioration of nerve cells releasing acetylcholine, a chemical

that helps to carry messages

among brain cells. The inadequate

supply of acetylcholine in

Alzheimerís patients is compounded by the action of an enzyme called acetylcholinesterase

(AChE), which breaks down acetylcholine in the body at the rapid

rate of 20,000 molecules per second.

The desired effect of potential

Alzheimerís treatments, such as

rivastigmine, is to inhibit AChE long

enough to offset the absence of

acetylcholine. But rivastigmine and

other anti-Alzheimerís drugs have

side effects and may merely slow

deterioration rather than halt it.

To look at the action of the drug

over time, Israel Silman, a neurochemist at the Weizmann Institute

of Science and a co-investigator on

the study, together with Pazit BarOn, a joint graduate student with

Sussman and Silman, tested the

drug on various types of AChE,

extracted from an electric ray, the

fruit fly, and human beings. ìWe

wanted to see how long it takes

AChEs to go back to normal, or

become ëreactivated,í after being

inhibited by the drug,î Silman says.

The scientists were very surprised

to notice an ìextremely low reactivationî of the AChEs from all three

organisms. ìInhibition of AChE by

rivastigmine appears to be almost

irreversible, with little reactivation

over a period of days,î Silman says.

To explain what happens at the

molecular level, the scientists took

ìsnapshotsî of rivastigmine while

it was binding to AChE, using a

method called x-ray crystallography. They projected x-rays produced at the NSLS on crystals of

rivastigmine combined with AChE.

They then determined the structure

of the complex rivastigmine-AChE

by looking at how the x-rays scattered off the crystal. By reconstructing the positions of these

scattered x-rays, the scientists established a molecular map that revealed the locations of all the atoms of AChE and rivastigmine in

three dimensions.

ìWhen we looked at this map,

things became clearer,î Sussman

says. ìWe had suspected that

rivastigmine was binding very

tightly to AChE, preventing surrounding fluid ñ mainly water ñ

from breaking this bond quickly, as

it usually does.î

By looking closely at the AChE ìactive siteî ñ the part to which

rivastigmine binds to AChE ñ

Sussman and his colleagues noticed that rivastigmine was broken

in two, each part being ensconced

comfortably in the active site (Figure 1). The scientists also precisely

determined how each part was

Joel Sussman Israel Silman
Feature Articles 2 - 54

Figure 1. Close-up view of how the drug rivastigmine binds to the active site of

the acetylcholinesterase (AChE) from the electric ray Torpedo californica. After

binding to the active site of AChE, the drug is broken into two parts, called

carbamyl moiety and NAP. Rivastigmine is rendered as a ball-and-stick model,

with carbon atoms colored yellow, oxygen atoms colored red, and nitrogen atoms

colored blue. Selected key molecules in the vicinity of rivastigmine are also

rendered in ball-and-stick format, with carbon atoms colored green.

Figure 2. Active site of acetylcholinesterase (AChE) from the electric ray Torpedo californica after AChE is inhibited by the

drug rivastigmine. Both parts of rivastigmine, the carbamyl moiety and NAP, are depicted with larger spheres and thicker

lines for emphasis. Amino acids within the active site of AChE that may interact with the drug are shown. The carbamyl

portion of rivastigmine is positioned to make two H-bonds (dashed lines) with the amide nitrogens of A201 and G119, as

well as non-bonded contacts (dotted lines) with F288 and F290. NAP, the second part of rivastigmine, makes H-bonds with

three water molecules (large red spheres) and the amide nitrogen of G118, as well as non-bonding contacts (dotted lines)

with W84 and F330. (A, F and G represent the amino acids alanine, phenylalanine and glycine, respectively).

bound to the surrounding AChE

atoms and moved other AChE atoms, which slowed down reactivation of AChE (Figure 2).

ìThe x-ray molecular maps allow

us to see how every atom of

rivastigmine interacts with the atoms of AChEís active site,î Silman

says. ìThis information will be important in designing new chemicals

that will target specific atomic sites

in AChE, possibly leading to better

drugs that last longer and have less

undesirable effects on Alzheimerís

patients.î

ìI am very excited by the perspectives offered by these results,î

Sussman says. ìBy fine-tuning the

properties of anti-Alzheimerís drugs

or their targets at the molecular

level, we can truly hope to find a

cure for Alzheimerís disease in the

future.î

BEAMLINE

X12C

PUBLICATION

P. Bar-On, et al., ìKinetic and Structural Studies on the Interaction of

Cholinesterases with the AntiAlzheimer Drug Rivastigmine,î Biochemistry, 41, 3555-3564 (2002).

 -Patrice Pages
2 - 55 Life Sciences

Infection with the human

papillomavirus (HPV) is the most

common sexually transmitted disease in the United States According to the Centers for Disease Control and Prevention in Atlanta,

Georgia, an estimated 20 million

Americans are currently infected ñ

but the vast majority does not

know it.

Though HPV sometimes causes

genital warts, in most cases, it infects people without causing visible symptoms. Women with persistent infections from certain types

of HPV are at risk for cervical cancer, as 99 percent of cervical cancers around the world are associated with HPV infection.

Preventing papillomavirus from

multiplying is one way of stopping

the infection. Toward that goal, a

team of scientists from Cold Spring

Harbor Laboratory (CSHL) in New

York, working at the National Synchrotron Light Source (NSLS) at

Brookhaven National Laboratory,

Scientists at NSLS Discover how Papillomavirus ëunzipsí DNA

Finding may lead to drugs to prevent sexually transmitted disease and cervical cancer

have gained new insight into how

papillomavirus ñ in this case, cow,

or bovine papillomavirus, commonly used as a model system ñ

starts to multiply, causing infection.

This new understanding could be

used to design drugs to stop HPV

infection, which is of particular significance since no cure or vaccine

are currently available, although

vaccine development is underway.

ìWe know very little about how

papillomavirus replicates,î says biologist Leemor Joshua-Tor, the Cold

Spring Harbor team leader. ìSo we

decided to look at the molecular

details of how the replication

mechanism is initiated, with the

aim of helping to design drugs that

act like monkey wrenches in the

replication process.î

 Like all viruses, a papillomavirus

is an infectious agent that uses the

cells it infects to reproduce itself.

Replication of HPV does not kill the

host cells, but can make them cancerous.

The infection process starts as follows: The papillomavirus first inserts its DNA ñ a double-stranded

helix containing the virusís genetic

information ñ into the host cell. The

virus hijacks the protein production

machinery of the host cell to produce a viral protein called E1. By

attaching to the viral DNA, E1 proteins can initiate the DNA replication process, so that more viruses

can be formed, and later multiply

further.

ìThe DNA double helix can be replicated only if it is ëunzipped,í which

allows proteins called DNA polymerases to make copies of each

strand,î Joshua-Tor explains. ìThe

E1 protein is known to initiate the

ëunzippingí process, but how it does

it is not very well understood.î

To look carefully at how E1 proteins

attach to viral DNA, Joshua-Tor and

her postdoctoral associate, Eric

Enemark, in collaboration with Arne

Stenlund, a renowned

papillomavirus expert at CSHL,

grew crystals of E1 and

papillomavirus DNA at two different stages of the attachment process, in which either two or four

E1 proteins bind to DNA.

The researchers then used a technique called x-ray crystallography

to determine the positions of the

atoms making up the E1 proteins

and DNA. X-rays produced by the

NSLS were projected toward the

crystals, and the positions of the

atoms were determined by looking

at how the x-rays scattered off the

crystal.

To their surprise, Joshua-Tor and

her colleagues observed that E1

uses two separate modules, one

shaped like a loop and the other

Authors of the study (from left to right): Leemor Joshua-Tor, Arne Stenlund and

Eric Enemark.
Feature Articles 2 - 56

like a helix, to bind DNA, each one

binding to a different DNA strand

(Figure 1). ìThis is very unusual,î

Joshua-Tor says. ìWe expected that

both modules would bind the two

strands simultaneously.î The scientists also noticed that the loop bind

more tightly than the helix, giving

loops a larger role in E1-DNA binding than helices.

When two E1 proteins attach the

DNA, Joshua-Tor and her collaborators observed that the loops bind

different strands (Figure 1). When

four proteins bind to DNA, they

form two pairs facing each other,

with proteins in each pair binding

the same DNA strand as the ones

on the opposite side (Figure 2).

These results suggested a mechanism by which the double-stranded

DNA might ëunzipí (Figure 3). ìWe

already know that, ultimately, the

unzipping process involves two

bundles of six E1 proteins each,

called hexamers, each ëunzippingí

the DNA in opposite directions,î

Joshua-Tor says. ìSo, we think that

the initial assembly of the two

Figure 3. Schematic representation of

how hexamers are formed and DNA

ëunzippingí process is initiated. (a)

When four E1 proteins bind to the

double stranded DNA (red and blue),

they link DNA strands with a separate

loop (yellow) that acts like a clip and

allows E1 to hold tight onto the strand.

Note that two proteins facing each other

hold onto the same strands: The blue

and red E1 proteins bind to the blue

DNA strand, while the purple and green

E1 proteins bind to the red DNA strand.

(b) The E1 proteins that face each other

(blue and red on one side, purple and

green on the other side) attach to each

other, and recruit four more E1 proteins

to form a hexamer on each side of the

DNA. The hexamers act like little

propellers moving in opposite directions

and ëunzippingí each DNA strand from

its partner.

Figure 1. Crystal structure of two E1 proteins binding to

papillomavirus DNA. Each E1 protein exhibits two modules:

a loop (yellow) and a helix (red), each binding to a separate

DNA strand, the loop binding more tightly than the helix

to the DNA strands.

Figure 2. Crystal structure of four E1 proteins binding

to papillomavirus DNA. The loops (yellow) of the two

proteins on the right (purple and green) bind one DNA

strand (pink), while the loops of the two proteins on the

left (red and blue) bind the other DNA strand (blue).

E1 E1

DNA

E1 E1

E1 E1

DNA

hexamers from the four proteins

shown in our structure is what

causes the strands to separate by

forming around the single strands.î

Joshua-Tor and her colleagues suggest that the four proteins separate into two pairs, each recruiting

four additional E1 proteins, thus

creating two hexamers that would

move in opposite directions (Figure 3). Each hexamer would encircle either strand, and act like a

little propeller that rotates around

the strand, thus ëunzippingí it from

its partner DNA strand along the

way.

ìIf this is the way these proteins

operate, it is pretty clever,î Joshua-
2 - 57 Life Sciences

Tor says. ìThis is the first time that

it has been found that the two individual DNA strands bind to two

separate protein modules prior to

the DNA ëunzippingí process.î

While Joshua-Tor and her colleagues are still investigating the

papillomavirus-induced DNA replication, they are also starting to test

compounds that interfere with

papillomavirus DNA replication. For

example, Anitra Auster, a graduate student, is developing compounds that could interfere with the

DNA replication induced by a highrisk type of human papillomavirus

that can lead to cervical cancer.

ìUnderstanding these binding

mechanisms could significantly

improve the treatment of this sexually transmitted disease,î JoshuaTor says. ìWe can now design and

test drugs aiming to prevent E1

proteins from attaching to the viral DNA, which is one of the first

steps to making much-needed

antivirals against HPV infections

and HPV-induced cervical cancer.î

BEAMLINE

X26C

PUBLICATION

E. Enemark, A. Stenlund, and L.

Joshua-Tor, ìCrystal Structures of

Two Intermediates in the Assembly of the Papillomavirus Replication Initiation Complex,î The EMBO

Journal, 21, 6, 1487-1496 (2002).

 -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - November

22, 2002.]
Feature Articles 2 - 58

For the first time, scientists have

observed the molecular details of

biological cells fusing together, a

fleeting event never before observed at this scale. This research,

which could lead to more efficient

drug delivery processes and

gene therapy techniques,

was performed on NSLS

beamline X21 and Rice University. The results appear

in the September 13, 2002

issue of Science.

Cellular membrane fusion is

well known to scientists and

is one of the most common

ways for molecules to enter

or exit cells, in processes

such as fertilization and viral infection. When two cells

fuse together, their membranes come together at

one location and create a

connection between the

cells that allows the exchange of material between

them. Eventually, the two

membranes form one single,

continuous membrane surrounding the contents of

both cells.

ìWe have now confirmed the

existence of a temporary

structure that occurs during

membrane fusion and that has

been postulated by scientists for a

long time,î says Lin Yang, a

postdoctoral physicist at the NSLS

and the lead author of the study.

Yang and coauthor Huey Huang,

professor of physics and astronomy

at Rice University in Houston, with

whom Yang did his doctoral studies, made their observation by serendipity while studying how certain

small proteins kill bacteria by digging holes into bacterial membranes.

Biological Serendipity: Molecular Details of Cell Membrane

Fusion Revealed

ìWe were trying to understand how

changes in humidity and temperature affect the properties of a certain type of cell membrane,î Yang

says, ìwhen, amid our results, we

observed this structure that nobody

had ever seen. That was pretty

exciting.î

To reveal the structure of the fused

cell membranes, the scientists used

a method called x-ray diffraction.

They first produced small crystals

composed of stacks of membranes

made of phospholipids. Then, they

projected x-rays produced by the

NSLS toward the crystals. By looking at how the x-rays scattered off

the crystals, Yang and Huang measured a pattern of points with varying intensities, called a diffraction

pattern, which represents a map

of the atomic structure of the phospholipid layers in the membranes.

ìWe noticed that by changing the

humidity, we could significantly alter the structure of

the membrane,î Yang says.

For certain humidity values,

the scientists noticed that,

instead of displaying a

single line of regularly

spaced points, the diffraction pattern revealed many

more points at other positions. By studying these diffraction patterns more

closely, the scientists realized that these patterns

were those of two membranes caught in the act of

fusing.

The diffraction pattern

showed that, when the two

membranes fuse, they form

an hourglass-shaped structure called a stalk, confirming theoretical predictions.

When the stalk stretches

further, it creates a connecting bridge between the

membranes. This connection then enlarges, and the

two membranes ultimately

become one single membrane.

Huang comments that the membrane considered in this study is

relatively simple and does not reflect the complexity of more common natural membranes, which are

made of phospholipids and proteins. ìWhat is truly exciting is that

we now have, for the first time, a

model system that can provide

clues about how more complicated

membranes work,î he says.

Lin Yang
2 - 59 Life Sciences

A simple representation of the fusion of two cells, with close-up views of the changes that the cellular membranes undergo.

Each membrane is made of a double layer of phospholipids which intermingle to create a passage between the cells. (Each

phospholipid is represented with a head and two tails.)

10nm

(Top) Diffraction patterns of two cell membranes before (left) and during (right)

fusion. (Bottom) Three-dimensional representation of the membranes before (left)

and during (right) fusion.

Understanding cell fusion may be

key to preventing viral infection or

designing new drug delivery methods, the scientists say. ìUnderstanding the details of membrane

fusion may help scientists find the

appropriate conditions for preventing viruses such as HIV from fusing to and thereby infecting human

cells,î Yang says. ìThis knowledge

could also lead to the design of

systems in which a drug or a piece

of DNA is enclosed in a membrane

known to fuse with specific cells in

our body, thus facilitating drug delivery or improving gene therapy.î

 ó Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - October 4,

2002.]
Feature Articles 2 - 60

Scientists working at the NSLS

beamline X25 have unveiled the

details of an important cancer protein. Though the protein, called Ski

- for Sloan Kettering Institute,

where it was identified in the early

1980s - is known to trigger tumor

growth, how it does this is still not

well understood. The new results,

which are reported in the November 1, 2002 issue of Cell, shed light

on this process and may provide

ways to design new anticancer

drugs.

ìWe now have a very important

clue as to how Ski interferes with

key proteins that prevent cells from

becoming cancerous,î says Yigong

Shi, a molecular biologist at

Princeton University. Shi leads one

of the two teams, one from

Princeton and one from Lawrence

Berkeley National Laboratory

(LBNL), that conducted the study,

Role of Cancer Protein Identified by Princeton, LBNL Teams at

NSLS

Yigong Shi

Schematic diagram of a proposed mechanism for the Ski-mediated repression of

TGF-fl signaling. By simultaneously binding to the cytoplasmic (yellow) and nuclear

(purple) signaling proteins, Ski prevents the two signaling proteins from binding

to each other, thus suppressing the action of TGF-fl.

Overall structure of the complex of Ski

and a nuclear signaling protein.

which is supported by the National

Institutes of Health and the Searle

Scholar and the Rita Allen Foundations.

ìUnderstanding how to stop Ski

from disrupting the normal function of cells will probably be key to

developing new anticancer drugs,î

continued Shi.

Ski prevents a protein called transforming growth factor-beta (TGFβ) from safeguarding cells against

excessive growth.

ìTGF-β acts like a molecular traffic

light, ordering certain cells to slow

down and stop dividing,î Shi says.

ìWhen TGF-β is blocked, for example by Ski, cells manage to

speed through this checkpoint, triggering runaway cellular growth that

eventually results in cancerous tumors.î

TGF-β cannot enter cells, so it

transmits its signal inside the cell

by attaching to receptor proteins

on the cellís outer surface. The signal generated by this interaction is

carried across the cell membrane

to proteins inside the cell.

Some of these signaling proteins

are triggered inside the cell cytoplasm and later bind to other proteins inside the nucleus. The combination of both types of signaling

proteins activates genes necessary

for the normal functioning of the

cell.

Ski, which is already present in the

human body, disrupts the signaling proteins when it is either

overexpressed or introduced by a

virus inside the body. The new
2 - 61 Life Sciences

study focused on the first of these

two possible processes.

ìScientists have previously shown

that Ski disrupts normal cell functioning by directly disrupting the

expression of genes inside the cellís

nucleus,î Shi says. ìBut nobody has

ever investigated whether Ski could

disrupt the signaling proteins that

activate the genes.î

The Princeton team looked at the

molecular details of a complex

made of Ski and nuclear signaling

proteins by using x-rays generated

at the NSLS.

The researchers saw that, as they

had suspected, Ski disrupts the

cytoplasmic signaling proteins, so

that when Ski binds to the nuclear

signaling proteins, the cytoplasmic

signaling proteins cannot attach to

their nuclear counterparts. ìThis

binding process is probably one of

the major ways in which Ski disrupts the signaling proteins and,

thus, suppress the action of TGFβ,î Shi says.

The LBNL team performed various

biochemical tests that confirmed

these results by also showing that

Ski binds to nuclear signaling proteins.

 -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - November

1, 2002.]
Feature Articles 2 - 62

Scientists at Johns Hopkins University in Baltimore, Maryland, have

provided new insight into the inner workings of a member of a family of proteins, called human epidermal growth factor receptors

(EGFRs), that are involved in abnormal tissue growth and cancer.

This research, which was performed at the NSLS could lead to

more efficient drugs aimed at preventing or treating some forms of

cancer. The results were reported

in the August 23, 2002 issue of

Science.

ìLittle is known about the structures of the EGFR family members,î

says Dan Leahy, a biophysicist at

the Howard Hughes Medical Institute (HHMI) and the lead author of

the study, ìyet they are involved

in many human cancers, including

breast, gastric, colon, and prostate

cancers. Our study is a starting

point to see how a possible drug

might help prevent or cure these

cancers.î

Scientists Uncover Molecular Clues About Origin of Cancer

Leahy and Hyun-Soo Cho, an HHMI

postdoctoral student, studied a

protein called human epidermal

growth factor receptor 3 (HER3),

which, like all the other EGFR proteins, is located on the surface of

human cells. When HER3 binds to

specific types of proteins, called

ligands, its shape changes, and

HER3 tells the cell to divide and

multiply.

Though HER3 is not known to be

involved in cancer, the abnormal

production of its close relative,

called HER2, is associated with particularly aggressive forms of breast

cancer. But attempts to study the

structure of HER2 have proven unsuccessful so far. Instead, by providing details of the molecular

mechanisms of HER3, Leahy and

Cho can now unveil some insight

into the inner workings of HER2.

ìIt is usually very difficult to determine the structure of EGFRs,î

Leahy says. ìIt took us more than

two years to get HER3ís structure,

and, now that we have it, it might

be easier to understand how its

relatives work.î

HER3 consists of three parts, which

are located outside the cell, in the

cell membrane, and inside the cell.

Leahy and Cho studied the outside

part of HER3, called sHER3, which

binds to specific ligands and

changes its shape during the binding process.

To reveal sHER3ís molecular details, the scientists used a method

called x-ray diffraction. They first

crystallized sHER3, and then bombarded the resulting crystal with xrays produced by the NSLS. By

looking at how the x-rays scattered

off the crystal, Leahy and Cho determined the positions of the atoms inside sHER3, thus establishing its three-dimensional structure.

The structure showed that sHER3

is made of four regions, and suggested how ligands attach to sHER3

and induce shape changes. One

unexpected aspect of the structure

is what the scientists call the ìsnapî

region ñ two finger-like loops that

reach out toward one another and

interact (Figure 1). Leahy and Cho

also noticed that the size of the

sHER3 binding site, which is comprised between regions I and III

(Figure 1), is twice as big as the

ligand size when the two finger-like

loops interact.

ìThe ësnapí region seems to prevent a ligand from binding,î Leahy

says. ìSo, the two finger-like loops

would have to detach from each

other to allow a ligand to bind to

sHER3, which informs the cell that

it can grow and divide.

ìIf future studies confirm that this

is how a ligand binds to sHER3,

then it is pretty exciting,î he adds.

ìThis means that we can now think

of new therapeutic approaches to

modulating ñ preventing or stimulating ñligand-binding to HER3 and

other members of the EGFR family.î

Leahy and Cho suggest two approaches to developing such modulation. In the first approach, intended to prevent ligand-binding,

the scientists propose to design

mutant forms of ligands that would

only bind to either region I or III,

but prevent normal ligands to bind

to HER3. As the finger-like loops

remain attached to each other, the

cell does not receive signals

prompting it to grow and divide.

In the second approach, Leahy and

Cho suggest to use molecules that

would affect the binding between

Dan Leahy
2 - 63 Life Sciences

the finger-like loops, by either

breaking or reinforcing this binding, and thus favoring or inhibiting

ligand-binding to HER3.

ìI am very excited by the therapeutic opportunities that can be

derived from the knowledge of the

three-dimensional structure of this

Figure 1. Ribbon diagram of the human epidermal growth factor 3 (HER3), showing domains I (blue), II (green), III

(yellow), and IV (red). Disulfide bonds are shown in purple and gold. The results of Leahy and Choís study indicate that a

ligand (left) may bind to HER3 when the ìsnapî region opens, which bends domain II to the left and brings domains I and

III close enough to ìtrapî the ligand between them.

N

C

“Snap”

I

II

III

IV

EGF

Binding

Site

receptor,î Leahy says. ìThis is just

the beginning, but I am confident

that similar studies will open more

possibilities of tailoring appropriate

drugs for the treatment of cancer.î

BEAMLINE:

X4A and X25

PUBLICATION:

Hyun-Soo Cho and Daniel J. Leahy,

ìStructure of the Extracellular Region of HER3 Reveals an

Interdomain Tether,î Science 297,

1330 (2002).

-Patrice Pages
2 - 65 Life Sciences

FUNDING

Department of Energy (DOE)

National Institutes of Health (NIH)

PUBLICATION

G. M. Dhavan, D. M. Crothers, M. R.

Chance, M. Brenowitz, "Concerted Binding

and Bending of DNA by Escherichia coli

Integration Host Factor," Journal of

Molecular Biology, 315, 1027-1037 (2002).

FOR MORE INFORMATION

Mark Chance, Professor of Physiology

and Biophysics, Albert Einstein College

of Medicine, Bronx, New York.

mrc@aecom.yu.edu

BEAMLINE

X28C

Integration Host Factor (IHF) is a

sequence-specific DNA binding protein that bends DNA and recognizes

several sites in the Escherichia coli

and lambda phage genomes. IHF's

ability to bend lambda phage DNA

makes it an important architectural

protein in the formation of a nucleoprotein complex that precedes the

integration of the phage into the

bacterial genome, as well as in several other biological processes.

The kinetics of IHF-DNA complex

formation affects the overall rate

of IHF-dependent biological process. In our work we have determined the site-specific association

kinetics of IHF binding to one of its

sites from the lambda phage genome, the H site. A key discovery

from our kinetic experiments is that

IHF binding and bending of DNA

happens in a concerted manner.

The IHF-DNA crystal structure

(Figure 1) was solved in 1996 by

University of Chicago's biochemist

Phoebe A. Rice and

her collaborators. We

conducted our timeresolved x-ray

footprinting experiments on this complex. Phosphorus(32)-radiolabeled

DNA was mixed with

IHF, the solution was

incubated, and later

exposed to NSLSgenerated x-ray

beams.

The cleaved fragments of DNA were

run on a denaturing

gel, as shown in Figure 2. The three protections along the

Host Factor and DNA in Escherichia coli

Mark Chance

Figure 1. The IHF-DNA crystal structure is shown

with the three sequence protein-DNA contact surfaces

observed in our kinetic study labeled A, B and C.

Kinetics of Association Between the Integration

G.M. Dhavan1, M. Brenowitz1, M.R. Chance1, and D.M. Crothers2

Scientists at the Albert Einstein College of Medicine in New York and

Yale University in New Haven, Connecticut, have conducted the first

analysis by synchrotron footprinting of the fast kinetics of a proteinDNA interaction. The work was conducted at NSLS beamline X28C, and

provided a detailed, single base-pair resolution of the exact points of

contact of a protein called Integration Host Factor on the DNA surface.

The scientists have shown that when protein and DNA samples are mixed

together, proteins capable of binding to DNA in a sequence-specific

manner yield protections against hydroxyl radical attack along the nucleic

acid surface. Two distinct phases are also observed in the association

process: an initial ìburstî phase, followed by a slower one.

1

Albert Einstein College of Medicine, Bronx, New York; 2Yale University, New Haven,

Connecticut

DNA correspond to the three contacts made by a single molecule of

IHF labeled A, B and C respectively.

A kinetic fit to the protections calculated for each site relative to a

control (unbound) DNA sequence

shows that the three 'footprints'

upon the DNA occur with similar

kinetics (Figure 3).

All three DNA binding sites are

bound by IHF with comparable kinetic profiles, indicating that they

are contacted concertedly in the

last step of IHF-DNA complex formation.

The best fit of the data to a bi-exponential equation is characterized
Science Highlights 2 - 66

by an initial burst phase in binding

that displays rates faster than the

speed of conventional diffusion

(around 109 M-1 sec-1) followed by

a slower phase in binding corresponding to a bimolecular association rate around 108 M-1 sec-1.

Figure 3. The kinetic curves obtained for each protection

pattern are shown as a least squares fit to a biexponential equation.

Figure 2. The image of the gel shown

contained separated DNA fragments during

complex formation for each time point (each

column). The developing protection patterns

as a function of time are labeled A, B and C

and correspond to the appropriate contacts

identified in the crystal structure.

The time-resolved x-ray

footprinting assay has also proved

extremely useful in determining

site-specific rates of RNA folding in

another nucleic acids kinetic study.

We envision that the set-up at our

committed beamline at the NSLS

will be instrumental in determining specific kinetics for individual

molecules in multi-protein-nucleic

acid complexes.
2 - 67 Life Sciences

FUNDING

Welch Foundation

National Institutes of Health

Human Frontier Science Program

Canadian Institutes of Health Research

PUBLICATION

A.D. Ferguson et al., ìStructural Basis of

Gating by the Outer Membrane Transporter FecA,î Science, 295, 1715 (2002).

FOR MORE INFORMATION

Andrew Ferguson and Johann

Deisenhofer: Department of Biochemistry, University of Texas Southwestern

Medical Center, Dallas

ferguson@hhmi.swmed.edu and

Johann.Deisenhofer@UTSouthwestern.edu

BEAMLINE

X12C

Structural Basis of Gating by the Outer

Membrane Transporter FecA

A.D. Ferguson1, B.S. Smith1, J. Deisenhofer1, R. Chakraborty2, L. Esser3 and D.

van der Helm4

1

Howard Hughes Medical Institute and Department of Biochemistry, University of Texas

Southwestern Medical Center in Dallas; 2Department of Health Sciences, College of Public

and Allied Health, East Tennessee State University in Johnson City; 3

Laboratory of Cell

Biology, National Cancer Institute, National Institutes of Health in Bethesda, Maryland;

4

Department of Biochemistry and Microbiology, University of Victoria in British Columbia,

Canada

Scientists working at the NSLS and Argonne National Laboratoryís Advanced Photon Source (APS) have determined the crystallographic structure of the outer membrane receptor FecA from Escherichia coli with

and without ferric citrate ñ an essential nutrient of bacteria ñ at 2.5 and

2.0 angstrom resolution. This study establishes the structural basis of

gating for receptors dependent on the cytoplasmic membrane protein

TonB.

Despite its relative abundance in

Earthís crust, iron is biologically unavailable in the atmosphere. So, in

response to iron deficiency, most

microbes secrete organic chelators

ñ compounds having a central metallic ion attached to two or more

nonmetallic atoms ñ called

siderophores, which are designed

to sequester ferric iron.

Bacteria survive by using highly

selective mechanisms designed to

actively pump iron across the cell

envelope. These mechanisms, responsive to both the internal and

external iron concentration, control

the transcription of genes involved

in iron uptake. The ferric citrate

uptake (fec) genes are responsible

for the transport of ferric citrate

from the external medium into the

cell. Embedded within the outer

membrane is FecA, a receptor that

binds and transports ferric citrate,

and is required to initiate transcription of the fec uptake genes.

We have determined the architecture of FecA from Escherichia coli

and its gating mechanism by x-ray

crystallography. Using mixed detergent-protein micelles, FecA crystals

with and without ferric citrate were

grown. Data was collected to 2.0 Å

Johann Deisenhofer, professor of

biochemistry and investigator in the

Howard Hughes Medical Institute at the

University of Texas Southwestern

Medical Center in Dallas, conducted the

study on the outer membrane

transporter FecA with lead author and

postdoctoral researcher Andrew

Ferguson. Deisenhofer received the

1988 Nobel Prize in Chemistry.

from unliganded FecA at beamline

X12C of the National Synchrotron

Light Source, and to 2.5 Å from

liganded FecA at the Argonne National Laboratoryís Advanced Photon Source.

FecA is composed of three domains

(Figure 1): (i) a 22-stranded antiparallel β-barrel embedded within

the outer membrane, with long extracellular loops and short

periplasmic turns; (ii) a ìplug,î consisting of a mixed four-stranded βsheet with short interspersed helices, and extracellular and

periplasmic pockets, located above

and below the plug; (iii) a disordered third domain, the NH2-terminal extension, which resides entirely within the periplasm and is

required for the initiation of transcription.

Ferric citrate binding affects the

conformation of the barrel and the

plug domain of FecA by causing a

dramatic change in the spatial arrangement and conformations of

primarily the seventh and eighth

extracellular loops, as shown in

Figure 2.

From our structural observations,

we propose the following transport

mechanism.

Stage 1: Ferric citrate is adsorbed

from the medium primarily by aromatic residues found within the

upper portion of the external

pocket of FecA.
Science Highlights 2 - 68

Stage 2: Ferric citrate is transferred to its high-affinity binding

site, causing an allosteric transition

within the plug that signals the occupancy of FecA in the periplasm.

Stage 3: Multiple extracellular

loops of the barrel change their

relative conformation and position,

thereby closing the external pocket

of the barrel.

Stage 4: Transitions that modify

the conformation of the plug domain and/or barrel are needed for

transport to occur, and are mediated by physical interactions between FecA and the cytoplasmic

membrane protein TonB.

Our findings clarify the current understanding of energy-dependent

siderophore uptake across the bacterial outer membrane, and establish the structural basis of gating

for TonB-dependent receptors. Further genetic and biophysical studies are needed to establish the

molecular basis of energy-dependent transport.

Figure 1: Crystallographic structure of FecA, (A)

unliganded, and (B) liganded. The 22-stranded β barrel

is shown in blue. The mixed four-stranded β sheet of

the plug domain is shown in green. The switch helix,

located in the periplasmic pocket of FecA, is colored

orange and is only observed in the unliganded

conformation.

Figure 2: Stereoview of the ferric citrate-binding site.

All side chains within 3.5 angstrom of dinuclear ferric

dicitrate are shown with carbon atoms in white, nitrogen

atoms in blue, and oxygen atoms in red. The strands

and extracellular loops of the barrel are shown in blue;

the strands forming the plug domain are in green, and

loops are in yellow. The dinuclear ferric citrate molecule

is represented with oxygen atoms in red, carbon atoms

in green, and ferric ions in orange.

A

B
2 - 69 Life Sciences

FUNDING

National Institutes of Health

National Science Foundation

Office of Naval Research

Deutsche Akademischer Austauschdienst

(Germany)

PUBLICATION

X. Chen et al., ìStructural Identification of

a Bacterial Quorum-sensing Signal

Containing Boron,î Nature , 415, 545

(2002).

FOR MORE INFORMATION

Fred Hughson, Princeton University

fhughson@molbio.Princeton.edu

BEAMLINE

X12C Structural Identification of a Bacterial Quorum

Sensing Signal Containing Boron

In a process known as quorum sensing, bacteria communicate with one

another using chemical signalling molecules called autoinducers. This

cell-cell communication allows a population of bacteria to coordinate

the gene expression, and therefore the behavior, of the group. Recent

work by researchers from Princeton University and the School of Chemistry, Polymers and Materials in Strasbourg, France, has led to the identification of a novel autoinducer, AI-2, that may serve as a ëuniversalí

signal for communication between different bacterial species. AI-2 unexpectedly contains boron, an element that, while ubiquitous in the

biosphere, has seldom been observed to play a role in biological processes.

X. Chen1, S. Schauder1, I. Pelczer1, B. L. Bassler1, F. M. Hughson1, N. Potier2, and

A. Van Dorsselaer2

1

Princeton University; 2Ecole de Chimie, PolymËres et MatÈriaux, Strasbourg, France

Quorum sensing allows a population of bacteria to coordinate their

gene expression, and therefore

their collective behavior. Usually,

quorum sensing controls processes

that are effective when a large

number of bacteria act together.

Some bacteria, for example, produce visible light in response to

autoinducers that accumulate in

dense cultures. Pathogenic bacteria can use quorum sensing to

evade the immune system, express

toxic virulence factors, or coordinate the formation of antibioticresistant biofilms.

Recently, we identified a novel

autoinducer, AI-2, that has the potential to mediate communication

among different bacterial species.

The presence of AI-2 can be detected by adding it to a specially

engineered strain of the bioluminescent marine bacterium V.

harveyi, which emits light in the

presence of AI-2. Using this assay, it was possible to show that a

large number of bacterial species

produce AI-2. These and other

findings suggest that communication via AI-2 could be a common

mechanism that bacteria employ

for inter-species interaction in

natural environments.

The chemical identity of AI-2 was

ascertained in a somewhat unusual

way using x-ray crystallography.

AI-2 was crystallized in a complex

with its V. harveyi receptor protein,

LuxP. Crystals formed by the LuxPAI-2 complex diffracted beyond 1.5

Å resolution at NSLS Beamline X12C. Because of the high quality

of the resulting electron density

maps, it was straightforward to

construct an atomic model for AI2 (Figure 1).

Earlier work had suggested that AI2 is derived from the precursor 4,5-

dihydroxy-2,3-pentanedione. The

cyclic form of this precursor is a

plausible substrate for the addition

of borate. We were nonetheless

surprised to find that the AI-2 electron density appears to match this

borate addition product. Confirmatory evidence, including 11B-NMR

spectra and the ability of boric acid

to stimulate bioluminescence in V.

harveyi supported the conclusion

that AI-2 is a novel furanosyl borate diester. Thus, interspecies

quorum sensing represents one of

the first biochemically defined roles

for boron in biology.

Many questions remain. For example, it is not yet clear how, or

whether, the use of boron enhances

signal transmission or signal specificity. Also, we do not yet know

whether the use of boron in cellcell signaling is confined to bacteria that live in marine environments

or is more widespread. Nonetheless, biotechnological research is

focused on the development of

molecules that are structurally related to AI-2. Such molecules may

be useful as anti-microbial drugs

aimed at bacteria that control virulence through AI-2 quorum sensing. Since many bacteria produce

AI-2, drugs that target AI-2 quorum sensing could be broadly used

in the future.

Members of the Princeton University team:

Team leader Fred Hughson (left) and

collaborator Bonnie Bassler.
Science Highlights 2 - 70

Figure 1. Structure of the LuxP-AI-2 complex. a. Electron density from which the LuxP contribution has been subtracted

to highlight the electron density for AI-2 in the center. b. Overview showing AI-2 (stick figure) bound to LuxP (ribbon).

The Lux P protein backbone is shown in rainbow colors from its N- to its C-terminus. c. Stereoview close-up of AI-2 bound

to LuxP, in the form of an electron density map (prior to AI-2 addition to the model). Boron, oxygen, nitrogen, and carbon

are colored yellow, red, blue, and gray, respectively.
 			




		
	
	

	






	
	

	




 !
"		

#$
	%
$%

	"		&%$'(	

$% )	

  *+*+,*--*.







"	
 /	
$	%

"%$$
% 0

1'	% 	 

"	"
2$

	

34

	 

	 	 

	 
	 	 

	 
	 	 


			


			
			


	
		
		
	

		
	



	
	
	
	
	

		


		

		

				
	



			 	
		

	
	!!	

		 		"		 	 !
	 	 !	


	 
	 
	 #	 $%&'	 	 (((	 )*+,$%&'(((-

.

	 	 /0	 1
	 	 
	 




		
	!	 	 	
	
	




	
				
	
	

		
	

 	 	 !	 
	 
	 	 	 	 	 



	

		


	
	








	



01'	% 	 

   	


  


				
	



 	 
 


	



	
					

		  
 
 			


	 	 

		
 			 

	


			

	


		
	
	

 	   !"# 
	$% 


	 	 


 	 
	


	
	


&  		
 




 	 
			

 

	 


 		



	$% 
	



  
 
  

	
	

'	
		


(	 )*+,  ---

. /0)*+,---1

   
 	 


 	 
	

		  



2	

		 




	
	

	
  


	

 
  


 
 
	


	) 2/,



'	



 

 

 /0)*+,--- 	  	 


	
	) /,
	


 (	 
 	

2  
 

 



	
		
(	



	
		

	


3

	



		    	 


 /
(	


	'
456


	

(	





	






'


476
486
	







 
 (	 
 

	 
	   9:3

	%	#



 ;	 #
  &
(

%	;










		 

  /0)*+,

--- 	   	
  
	

		
 
 <	


	 		
 
 	
	

		



 
	
	 ( 	

	
 	 
 	



 
	
 #
 

 /0)*+,--- 			 	
	

(	


	

 
 	 
  &


 3 
 
	
  

		
	
	


	 
&
 
3<	

	


  			 	
	

( 	 
 

	

	 
			 	

		
	
	

2


 /0)*+,

--- 
	
 
	 

		
  



 	


	 
	 	

 /0)*+,--- ' 	


  	
	 ( 

 /0)*+,--- 

				


	


	 
 	   
	

		
 

		

 !!!"#$%!!!& '(



	
)*+



(





#$%!!!

 

%
  


	  
 
   	 	, 
	   	

 
, 
	

 
	
	


 

 
	  
 

 	
 )	 	 	



			
,
	

	
	 	 

 



 
 

 
 


 
 2	  

		
  	
  

 	   
	  

	
 /0)*+,---	

 		 
 
 


		


2		

	


	 	  /0)*+,---


	



			


!"#$% <


				
	( /0)*+,

---

	 	
	


	
	=2
	

			
	


'

	
				


2	 
	
  	


	 
  
	  


	 		
  

	
	
	

  
		
  /0)*+,---


 

 			 
	



2 - 73 Life Sciences

FUNDING

Chemical and Biological Non-proliferation

Program of the U.S. DOE

U.S. Army Medical Research Acquisition

Activity

PUBLICATION

S. Eswaramoorthy, D. Kumaran and S.

Swaminathan, ìA Novel Mechanism for

Clostridium botulinum Neurotoxin

Inhibition,î Biochemistry, 41, 9795-9802

(2002).

FOR MORE INFORMATION

Subramanyam Swaminathan, Biology

Department, BNL, Upton, New York

swami@bnl.gov

BEAMLINE

X12C

The bacterium Clostridium botulinum produces one of the most potent neurotoxins ñ poisonous proteins acting on the nervous system

ñ to humans. Seven different types

of neurotoxins, labeled A to G, are

produced by the bacterium.

To infect a neuronal cell, a neurotoxin first binds to the membrane

of the cell. Then, the cell membrane

curves inward, incorporating the

toxin into a vesicle that drifts inside the cell. The toxin escapes the

vesicle by creating a channel in the

vesicle membrane, inserting its

light chain (LC) through the channel, and slipping away completely

into the cellís cytosol (fluid portion

of the cytoplasm). The toxin is

ìtranslocatedî from the vesicle to

the cytosol. Then, the toxin cleaves

specific targets in the cytosol and

blocks the release of neurotransmitters ñ chemicals produced by

neurons to communicate with each

other ñ thereby causing muscular

paralysis and the eventual death

of the patient infected with the bacterium.

The three-dimensional structure of

a botulinum toxin reveals three

domains, called binding, translocation, and catalytic domains, correA Novel Mechanism for Clostridium Botulinum

Neurotoxin Inhibition

Treatment of botulism, an acute paralytic disease caused by the bacterium Clostridium botulinum, is currently only preventive. An experimental

vaccine is available, but no drug has been developed yet. Biologists at

Brookhaven National Laboratory are studying how a chemical called

bis(5-amidino-2-benzimidazolyl)methane (BABIM) inhibits one of the

toxins produced by the bacterium. The results of this study could help

design new drugs against botulism.

sponding to the three functions of

the toxins.

All seven toxins contain a zincbased structure in their catalytic

domain, but structural details may

be different, because each toxin

cleaves different types of targets.

For example, the catalytic zinc is

located in a deep cavity in the active site of all toxins, but the cavity is partially covered by a ìbeltî

region in botulinum neurotoxin A

(BoNT/A) while it is open in BoNT/B.

Treatment of botulism is currently

only preventive: An experimental

vaccine is available, but no drug

has been developed yet. Therapeutic treatment could be effective at

any one of the three stages of toxicity ñ binding of toxin, internalization, or catalytic activity.

Chemicals such as Bis(5-amidino2-benzimidazolyl)methane

(BABIM) are known to combine

with the catalytic zinc, thus preventing the toxin from binding to

specific targets, also called substrates, in the cytosol. But the effectiveness of BABIM on the toxin

needs to be further investigated.

We have determined the crystal

structure of a complex of BoNT/B

and BABIM, and investigated how

BABIM binds to the zinc atom and

inhibits the toxin.

The crystal structure of the complex revealed a tunnel that connects a cleft formed between the

translocation domain and the catalytic domain to the active site cavity, as shown in Figure 1.

S. Eswaramoorthy, D. Kumaran, and S. Swaminathan

Biology Department, Brookhaven National Laboratory, Upton, New York

Authors of the study (left to right): Subramaniam Eswaramoorthy

(lead author), Subramanyam Swaminathan, and Desigan Kumaran.
Science Highlights 2 - 74

Interestingly, two molecules of

BABIM bind to the toxin on either

side of an aspartic acid molecule,

suggesting that the inhibitor can

enter and bind to the active site in

two different ways. We suggest that

one inhibitor molecule has entered

through the cleft between the

translocation and catalytic domains

while the other has entered through

the wide opening of the active site

cavity.

The inhibitor molecule near the

active site perturbs and disrupts

the zinc bonds to surrounding molecules in the toxin, as shown in

Figure 2.

The structure of the BoNT/B-BABIM

complex has shown that the active

site residues rearrange in the presence of the inhibitor, allowing it to

partly occupy the site where the

substrate would bind. Also, the zinc

atom is progressively removed

from the active site and transported to a different site in the protein. We have also shown that it is

possible for appropriate inhibitors

to enter the active site of the toxin

contrary to the belief that the belt

surrounding the catalytic domain

shields the active site. But the inhibition could be due to either the

non-availability of substrate-binding sites, the removal of the zinc

atom, or a combination of both.

Figure 1. Representation of the electrostatic

potential surface of botulinum neurotoxin B. The

two molecules of bis(5-amidino-2-

benzimidazolyl)methane that are trapped in the

tunnel and the residues coordinating the zinc

atom are shown as sphere model. Zinc atoms

are shown in yellow while water molecules

coordinating with the zinc atoms are in silver

gray.

Figure 2. Representation of bis(5-amidino-2-

benzimidazolyl)methane (BABIM) at the

neurotoxinís active site, with the light chain and

the belt region. Coordination to the zinc atom

from protein ligands and BABIM are shown as

thin yellow lines.
 			




	












	



 !" #
 $%
 %

&'( )$*+",

-



))

.  

 /012,/011324425







)$ 


 



$
 6

7


8
,


	

90

	 
	 
	 	 	 	 	 	 	 
	 	 



	

									

	 	 
	  	 	 	 

	 
	 !	 

		
	
		
	"

	#
		


	 $
	 %&	 
	 	 '
	 (
	 )	 *	 	 #



	 	 
	 	 	 	 	 	 &	 





	 

	 	 	 

	 +#,!,-	 


+#,-		

	
	
		


		
	'
		

	
				


	



	



		
		

 		
 
  




		


	












  !   




	





"	

	
#


	

	




"  	
 

 


$
	%		







"	
 "	&


 
 " '  


(!




   ! 
	

"	



"	





)

 

 
 







  
	
		

		



*
+,
	



"



-.

%


 &
 &'
  &' /



		"








)



&'





-0



			


1)	


"


/1
2&

)  (
	""
 	  


3	( 



	
 4
 5#
 

 
		

 
 " 

 
   
 

&'

/ 5# 
" 
"  


 #
 

"

 (6!
 		 "



 
  &'


  !
   "7"

		  8	2!
 


  	 	 

&' 

 5#   
	

	" 
  8	2 
"	

  &'
 

	


		 
 
 
 





/



&'
 
 
 

""


	

	

 (
"/
 



   
 


		
 

  

 
	    	

" 9(	  6!21: 


	)
0;;
 <!

0=<
	"
)	

/ 0;; < 
	"


	 "" 

)	  % 
 

""
/3

	
	>""0;

	 	!

	
	

	
	
	

	

67
 $:
6

 	 
 
 

 


 
 
 
 	 	
 










!"#$


"
%&


		
 

/ &'
 
 


		
	
	



 
  	
  
   		

#
		

?
	




	
"

&'



  	


"	@ ,"" ,
;!


	;
%	
  


%	


"


	




	 
!

A 
  
	 




&'









"








	

 -- 		 



 


"

 	 

 	 
 '!(


)*!

 
	 
 +
 	 ,(


(,)-)( (-(
.




 
 
 
 	 
 *
 

 	 	 



$(

 	    
 
 / 








 
 
(, 
 
 



*&
. 

	)

	

	




$




	
 .
   0 


0
/

	
'!(




(
(
$












.

2 - 77 Life Sciences

FUNDING

The Robert A. Welch Foundation

National Institutes of Health

PUBLICATION

T. Zhou, et al., ìStructure of Human

Nicotinamide/Nicotinic Acid Mononucleotide Adenylyltransferase: Basis for the

Dual Substrate Specificity and Activation

of the Oncolytic Agent Tiazofurin,î J. Biol.

Chem., 277, 13148-13154 (2002).

FOR MORE INFORMATION

Hong Zhang, Assistant Professor,

Department of Biochemistry, University of Texas Southwestern Medical

Center, Dallas, Texas

zhang@chop.swmed.edu

BEAMLINE

X12B

Nicotinamide adenine dinucleotide

(NAD) is a coenzyme (nonprotein

part of an enzyme) that has been

known for decades as the major

hydrogen donor or acceptor in

many metabolic reactions inside

the cell, as well as the modification of nuclear proteins by ADP

ribosylation, a process involved in

DNA repair and the regulation of

genomic instability.

Scientists have recently found that

NAD is a substrate or a co-factor

in the SIR2-like histone

deacetylase, responsible for gene silencing

and the increase of

lifespan of many species, including yeast,

worms, and mammals.

Also, several derivatives of NAD are intracellular calcium mobilizing agents in various

calcium signaling pathways.

NAD results from the

addition of adenylate

(one of RNAís building

blocks) to the molecule

nicotinamide mononucleotide (NMN), a

process catalyzed by

Structure of Human Nicotinamide/Nicotinic Acid

Mononucleotide Adenylyltransferase (NMNAT)

Nicotinamide adenine dinucleotide (NAD) is a coenzyme (nonprotein

part of an enzyme) involved in many metabolic reactions inside the cell,

as well as DNA repair and calcium signaling. NAD results from the addition of adenylate (one of RNAís building blocks) to the molecule nicotinamide mononucleotide (NMN), a process catalyzed by the enzyme NMN

adenylyltransferase (NMNAT). The enzyme is also involved in activating

the anticancer agent, tiazofurin. To understand better the role of NMNAT

in NAD biosynthesis and tiazofurin conversion, scientists have used xrays produced at the National Synchrotron Light Source and the Advanced Photon Source to determine the structure of NMNAT with different ligands, providing insight into the molecular mechanisms of the

enzymeís active site.

the enzyme NMN

adenylyltransferase (NMNAT). NAD

can also be synthesized by the following two successive processes:

addition of adenylate to the molecule nicotinate mononucleotide

(NaMN), leading to nicotinate adenine dinucleotide (NaAD), and

addition of an amide group (organic

compound containing the CONH2

radical) to NaAD, leading to NAD.

The first process is catalyzed by

NMNAT and the second by NAD

synthetase. (A synthetase is an

enzyme that catalyzes the union of

two molecules.) The processes are

illustrated at:

http://hhmi.swmed.edu/Labs/hz/

nad1.htm

Human NMNAT also catalyzes part

of the metabolic conversion of the

anti-cancer agent, tiazofurin, to its

active form, tiazofurin adenine dinucleotide (TAD), an NAD analogue. The development of

tiazofurin resistance has been

shown to relate mainly to a decrease in NMNAT activity. The process is illustrated at: http://

hhmi.swmed.edu/

Labs/hz/tiazofurin.htm

Human NMNAT, located within the cell

nucleus, recognizes

both NMN and NaMN

substrates. To understand the enzymatic

properties of NMNAT

and how its activity is

regulated, we have

solved the crystal

structures of human

NMNAT attached to

several ligands, including NAD, NaAD, and

TAD, to 2.2-angstrom

(Å) resolution.

T. Zhou1, D.R. Tomchick1, D.D. Binns1. N.V. Grishin1, H. Zhang1, O. V. Kurnasov2,

A.L. Osterman2, and V.E. Marquez3

1

Univ. of Texas Southwestern Medical Center at Dallas; 2Integrated Genomics, Inc.; 3

Frederick Cancer Research and Development Center, National Cancer Institute

Hong Zhang (lead author, right) and two members of her team:

Subramanian Karthikeyan (seated) and Xuejun Zhang, at the

University of Texas Southwestern Medical Center in Dallas.
Science Highlights 2 - 78

Figure 1. Left: Ribbon diagram of human nicotinamide mononucleotide adenylyltransferase (NMNAT) hexamer. Right:

The active site of human NMNAT with nicotinamide adenine dinucleotide (NAD) and nicotinate adenine dinucleotide (NaAD).

A water molecule (denoted w1) in the active site of NMNAT changes location upon binding to different substrates.

The data were produced and collected by using x-rays at beamline

X12B of the National Synchrotron

Light Source and beamline 19ID of

the Advanced Photon Source at

Argonne National Laboratory.

Our results show that NMNAT bind

to NMN and NaMN with high affinity. In particular, a water molecule

in the active site appears to play a

critical role in the recognition of

NaMN (Figure 1).

By looking at the structure of

NMNAT attached to TAD, we found

that TAD molecule adopts a similar

conformation as the native ligand

NAD, and that TAD and NAD form

essentially the same interactions

with NMNAT. Additional functional

groups on tiazofurin molecule also

may enable more favorable interactions between tiazofurin and

NMNAT. Further kinetic measurement will be needed to fully characterize the molecular interactions

between human NMNAT and

tiazofurin.

The results presented here represent a first step in our effort to decipher the metabolic pathways of

NAD biosynthesis and how it is

regulated in humans. We have recently identified an additional cytosolic form (inside the cell cytoplasm instead of the cell nucleus)

of human NMNAT; its structural determination is well underway.
 			




	



	







 !"#$%

&




#'	
  ()*(+()*,

-.))./







&
0%
#1

	



%%
	1




2


	

34

 	
 	 
 	


		
	


	

	
			

	  	


	 	
 	
		 

	
	
			


  		 	
 	 

 		   

	
!	

	 
  		 

	
  	 
 	 

		    	  

	"		

	  
	
	 

 	 		 			  	


  "		 	



#

			 

	

$		 
  	

	 
	 		 % 	


	

 	  

 
	
	 

	 	 %&  	

	   '	 

	 	 	 "


		
	

		

	
	

( 	
  	 	

	
		

)	
	

	

	
			


	




	


		
				




	  
 	

	 

  

 
 

	

 




	!		 

!		


	

	
	




" 



	

	#
	
$
	
%	$

	
	
&

		
		


'			



	


	
	
	
	

	()
	

		*



	+
	&
	


	

		


	
,

	









				

  
 	
 

	
	

	

#		 	 

		 
 

	
 	
  		

		*

	
 	 


	
 	 	
	 	

	  	 		 "

		 	 		
 	

		*



 
  
	 #

					
	
"

   		  	

	

 	 	 	  #


		"		

			"		 		

   

	
  	 +

$ , $	 

)	+,

	 	  #  	

		 		 )	 		
	  	

  
   	


 -

.    " 

	
	
	

 ( 			
 

"		
	

	
			


		

	

				

	

0%
#1
#5		

%%
	1

	





		
 

/  	  		

 -,				


 		 	 		

	"
		

				"			

 	    *	


 
	 		  		

	
		
	


	 
 


"		  	 		
	

			"

	 	   	 
	


	

0   
   


)				"#

1				

			
 
	
	

!	 	"#

	!!	"
"


#

	$	


			


%	
&


$ 	  	 #   	 	 	!" 
%
# 	 	  !# 	$  

	!	 "
	
#	

!

		!		!##	
#	#

							 

  	
   

	%	
	
234

  	 	  	

					 

		

#

						

			


			


	#


	

	
	")

	 	 	 


	
	

	


-

	,		
#	


5"5	1	(

	
  (	  	


	

6
- 		7		

#&		
#	


 5"5	1	

(	
  (	 

	
	

6
- 		7		
2 - 81 Life Sciences

FUNDING

National Institutes of Health

R. Welch Foundation

PUBLICATION

H. Jayaram, Z. Taraporewala, J.T. Patton,

and B.V.V. Prasad, ìRotavirus Protein

Involved in Genome Replication and

Packaging Exhibits a HIT-like fold,î Nature,

417, 311-5 (2002).

FOR MORE INFORMATION

B.V.V. Prasad, Prof. of Biochemistry,Verna

and Marrs Mclean Department of

Biochemistry and Molecular Biology,

Baylor College of Medicine, Houston,

Texas

vprasad@bcm.tmc.edu

BEAMLINE

X8C

Rotavirus, the leading cause of infantile gastroenteritis, with nearly

a million deaths worldwide every

year, has a spherical shape with

many spikes that bind firmly to a

host cell. The virus is composed of

six structural proteins arranged in

three concentric layers, which enclose the viral genome consisting of 11 doublestranded RNA (dsRNA) segments. Each segment codes

for at least one protein, except for one segment that

codes for two proteins.

Every rotavirus particle is a

fully contained unit that

transcribes genome segments from the inside, and

then releases the resulting

messenger RNA (mRNA)

molecules. When a

rotavirus fully replicates its

genome, several copies of

the 11 segments are made

(genome replication), and

each progeny virus gets one

copy of each segment (genome packaging).

One of the least understood,

yet critically important, processes in the replication

process of a dsRNA virus is

X-ray Structure of the Rotavirus Protein

Involved in Genome Replication and Packaging

H. Jayaram*, Z. TaraporewalaÜ, J. T. PattonÜ and B. V. Venkataram Prasad*

*

Program in Structural and Computational Biology and Molecular Biophysics, Verna and

Marrs McLean Department of Biochemistry and Molecular Biology, Baylor College of

Medicine, Houston, Texas; Ü

Laboratory of Infectious Diseases, National Institutes of Allergy

and Infectious Diseases, National Institutes of Health, Bethesda, Maryland

Using x-rays at beamline X8C of the National Synchrotron Light Source,

scientists have determined, to 2.6 angstrom (tenth of a billionth of a

meter) resolution, the first x-ray structure of a key protein, called nonstructural protein 2 (NSP2) of a rotavirus, the major cause of life-threatening infantile gastroenteritis. The structure provides molecular details

of the proteinís doughnut-shaped functional part, and reveals how it

may be involved in the replication and packaging of the viral RNA during

infection.

J. Patton (left) and Z. Tarporewala

H. Jayaram (left) and B.V.V. Prasad

the genome replication and packaging. The process by which the

correct set of dsRNA segments is

assigned to the capsids of each

progeny virus remains a mystery.

Several in vivo and in vitro studies

on rotavirus have provided insight

into the role of proteins that are

not incorporated into the virus but

merely assist in genome replication

and packaging. These proteins, referred to as non-structural proteins

2 and 5 (NSP2 and NSP5), are colocalized, along with the viral RNA

polymerase, called VP1, in granular cytoplasmic inclusions, or

viroplasms, in the infected

host cell. (The RNA polymerase is the main protein

involved in RNA replication.)

Recent biochemical studies

have shown that NSP2ís

functional part, a doughnutshaped octamer ñ containing eight repeating units, or

monomers ñ binds to RNA,

has a nucleoside triphosphatase (NTPase) activity

and has nucleic acid destabilizing activity. Based on

these studies, NSP2 is

thought to work as a molecular motor involved in genome

packaging, by using the energy derived from the hydrolysis of nucleoside triphosphates.

We have determined the

crystal structure of the functional octamer of NSP2 to a
Science Highlights 2 - 82

resolution of 2.6 angstrom (tenth

of a billionth of a meter) resolution

(Figure 1). Our studies have provided a firm ground to develop a

mechanistic understanding of how

NSP2, in concert with NSP5 and

VP1, may facilitate genome replication and packaging.

The structure of the NSP2 monomer (Figure 2) displays two distinct domains: an amino-terminal

domain and a carboxyl-terminal domain. A characteristic feature of the

monomer is a 25-angstrom deep

cleft between both domains.

While the amino-terminal domain

exhibits a fold not seen in any other

protein as yet, the carboxyl-terminal domain surprisingly, despite

any noticeable sequence homology, exhibits a fold that is observed

in the Histidine Triad proteins, a

family of ubiquitous cellular proteins that hydrolyze nucleotides.

This suggests that the cleft in NSP2

might correspond to the active site

for NTP hydrolysis.

The RNA binding and nucleic acid

helix destabilizing activities of NSP2

may require the formation of the

octamer. In particular, prominent

grooves, lined by positivelycharged residues, at the sides of

the octamer are ideal for binding

to single-stranded RNA. The proposed NTP binding sites are located

on either side of the groove.

Although NTP hydrolysis is not directly linked to either the RNA binding or the helix destabilizing activity of NSP2, nucleotide binding into

the cleft may alter the conformation of the monomer and affect

octamer-RNA interactions. Such

changes may facilitate transfer of

the bound RNA through the polymerase during replication, resulting in concurrent synthesis of duplex RNA and its packaging into

assembling progenitor viruses.

Figure 2. X-ray structure of the

monomeric subunit of the nonstructural protein 2 (NSP2). The aminoand carboxyl-terminal domains are

shown in green and red, respectively.

The cleft between the domains is

indicated by an arrow.

Figure 1. Surface representations of the octameric part of the non-structural

protein 2 (NSP2). (Left): View along the 4-fold axis of the octamerís 4-2-2

symmetry. (Right): View along one of the 2-fold axes. The groove in the octamer

is shown by a pair of arrows.
Surfaces, Interfaces

and Nanomaterials
 	

	







	


		
	

		
	
					

		

			
	
	

	 	 
	 	 






	 
	 
	 	 	 	 



	 	 
	 
	 


	 

		
				
		




		
	


 	


	 


	 	 

 	 	 



		
	

 	


	

		


	


	



!
	"

#		
		


	


	$	%
 	&


'()		
	


	


		
	


		


	

		
	


		

		
			




	 

	 	 

	



	
		
	

		




 	 	 	  	 	 


	
 	
	
	


	
	
	

		


				

		



	




*	
 	
	
		
		




	
	
	


 		



	

	
	


	


						


	 +
 	 
	 
	 	 




	 

	 	 
	 




	"!
	
	
	


	

	
	
	


	
	 
		 	

	 



	
	

		


	 	 
	 
	 

 #

%
	



!
	 


	 
	 
	 
	 





	
	
	
	
 

		

	
	!
	
 


	
	

		
 


	 	 
	 	 	 




	 


"
	 	 	 
	 
	 


					


		


			
	 #	



%
	"
	


		
	


	 	 


 	 
	 

	 



	 	 
	 	 


	
#

	 
	 




	 
	 


	
		


		




	
	

	 		




"
	

	 	


	

	


	)
		,	
	

	


	

 #	%
	



	
			 
	




				
		



	
 		
	

	


"
	 	
 	 
	 
	 




	 
	 	 
 	  


			
	
	
 


		

	
	

 	(

	 	 
	 	 
	 
 	 



	 	 	 	 
	  #

%
	 

	 "
	 
	 	 	 



			

	
		


			

			




 	 

	 	 


	 


			
	
		


	
#

%
		
	


	
	



	 	 	 

	 	 

	 



		
		


		


	



	

		!
	
 

	

		

	
	



	


 	
		



	 


"-

	 	 
	 


	 


	
 	
	
	
	



	
			
	
 #

'()	 

	 "-	 	 
	 




	 	 
	 
	 




	 	 


	 

 

	 	 
	 
	 




		
	




#	!
	



	
	



	

		

	


		
	
	




*		

	
	
	




	 


	 
	 





	 	 
	 	 

	 




"!
	


	


		


	
	
	

			




	
	
 #	



%
	" 	
				



	






 

								

		 !				

   				 	   " #$  	

%&			'	%	' 


	 	 
	 	 	 




 	
	

	


	



	
	
	

	





	 
	 
	 	 	 


		
	

	

 	



		




".	 

	 
 	 	 
	 
	 



 #	 
	 
	 "!
	 

	 




	 	 

	 
	 
	 


	 	 


	 
	 


	  	 
	 	 	 	 




		

		
 	




	
	
	
/

)
		



	 	 
	 	 	 



 	 
	 

	 
	 




#

%
	 
	 
	 


	 "

		
#	!
	






			
	

	


		
	
	



	 	 	 

	 

	 


	
			




		


		




																												0
	0



()*+,-

  ./0.-1	2

3443 5
2 - 85 Surfaces, Interfaces, and Nanomaterials

Scientists Create New Material With Varying Densities of Gold

For the first time, scientists have

created a material with a gradient

of gold nanoparticles on a silica

covered silicon surface using a

molecular template. The material,

which was developed at North

Carolina State University (NCSU)

and tested at the NSLS, provides

the first evidence that

nanoparticles ó each about one

thousand times smaller than the

diameter of a human hair ó can

form a gradient of decreasing concentration along a surface. A description of the material appears as

the cover story in the July 23, 2002

issue of Langmuir.

ìThis material promises to be the

first in a series with many applications in electronics, chemistry, and

the life sciences,î said Rajendra

Bhat, a Ph.D. student from NCSU

and the lead author of the study.

Bhat worked with Jan Genzer, a

chemical engineering professor at

NCSU, and Daniel Fischer, a physicist from the National Institute of

Standards and Technology (NIST).

To build the material, the scientists

first prepared a very thin layer of

organosilanes, sticky molecules

with a head and a tail, on a rectangular surface of silica.

ìThe head glues to the surface,

while the tail sticks out, acting like

a hook waiting for a gold

nanoparticle to attach to it,î explained Genzer, leader of the NCSU

team. The molecules, emitted vertically in the form of a vapor by a

source close to one side of the surface, slowly fell on it with decreasing concentration as the distance

from the source increased, thus

creating a gradient to serve as a

Material could be used to make better filters, more efficient sensors, and

Nanoparticles

faster catalysts

molecular template.

The next step was to dip the material in a solution containing the gold

nanoparticles, each of which was

coated with a negatively charged

chemical. In the solution, the tails

of the organosilane molecules took

on a positive charge, so the negatively charged gold particles attached to the oppositely charged

tails underneath.

To visualize the gradient of gold

particles, Bhat and his colleagues

used an atomic force microscope,

in which a tiny needle moves along

the surface, following its bumps

Images of gold nanoparticles attached to the silica surface at different distances

from the most populated end of the substrate. As the distance increases, the

number of particles decreases, revealing a particle gradient. Bottom: Simplified

representation of the material showing particles in decreasing concentration along

the surface.

Jan Genzer Rajendra Bhat Dan Fischer
Feature Articles 2 - 86

and valleys to reveal its topography. To look at the gradient of the

organosilane molecules, the scientists used a technique called nearedge x-ray absorption fine structure (NEXAFS). In NEXAFS, extremely intense x-ray light is sent

toward the material, and the electrons emitted by the material and

collected with a sensitive detector

provide information about the concentration of the organosilane molecules on the surface.

ìWe needed to confirm that both

the gold particles and the sticky

groups followed the same underlying gradient template,î Bhat said.

ìThe results from both techniques

were expected to coincide if the

particles were attaching to the underlying layer of sticky molecules.

Our results show exactly that.î

ìThe distinguishing feature of our

approach is that the particles follow a pre-designed chemical template provided by the organosilane

sticky groups,î said Genzer. ìThe

ability to manipulate the underlying template allows us to prepare

gradient structures of nanoparticles

with varying characteristics.î

The main advantage of the gradient structure is that large numbers

of structures can be combined on

a single substrate and used for

high-throughput processing. It

might, for example, save time for

chemists testing clusters of

nanoparticles used as catalysts ó

chemicals actively sought by the

chemical industry to create new,

less polluting sources of energy.

ìClusters made of different numbers of nanoparticles could be put

on a single surface, and scientists

could test this surface only once in

a chemical reaction, instead of having to run each cluster separately

through the reaction,î Fischer said.

The material could also be used as

a sensor to detect species that have

specific affinities for nanoparticles,

or as a filter to select particles of

given sizes.

Bhat and his colleagues are now

exploring the properties of similar

materials, with different ìstickyî

substances and nanoparticles.

ìThis research is so new that we

are still thinking of potential applications for these materials,î he

said.

 -Patrice Pages
2 - 87 Surfaces, Interfaces, and Nanomaterials

Understanding the properties of

nanoscale materials may allow scientists to manipulate these properties to produce new

nanomagnets, nanocatalysts, and

composites with better optical

properties. But such applications

require detailed knowledge of the

materialsí atomic level structure.

ìWithout a structure, you are without a road map,î said Thomas Vogt,

BNL Physics Department. Funded

by DOEís Office of Basic Energy Science and the National Science

Foundation, Vogt and scientists

from Michigan State University

(MSU), led by MSU physicist Valeri

Petkov, have demonstrated a technique that allows them to decipher

Nanoscale Crystallography Reveals Structural Details

Tom Vogt of BNLís Physics Department illustrates the

location of a cesium atom (golf ball) in the nanopores of

a zeolite ó a structure determined using methods of

nanocrystallography

such fine-level nanostructures.

The researchersí analysis of a material composed of cesium ions

trapped inside nano-sized pores of

the silicon-oxide zeolite Si 32O64 is

described in Physical Review Letters of August 12, 2002. This material is also the first example of a

room-temperature inorganic

ìelectride,î a stable separation of

positively charged cations and electrons, with properties determined

by the topology of the pores in the

host matrix.

Nanoscale structures ó made of

particles 1,000 times smaller than

the diameter of a human hair ó

are so difficult to decipher because

they lack the long-range order and

symmetry of perfectly crystalline

materials.

ìThis work shows that, even with

a very low degree of order, at synchrotrons such as the NSLS, and

using the right techniques, we can

determine nanoscale structures.

And with structural understanding,

we can begin to predict properties,

and perhaps begin to manipulate

them for useful applications,î said

Vogt.

 -Karen McNulty Walsh

[Editorís note: Reprinted with permission from the BNL Bulletin - October

18, 2002.]
Feature Articles 2 - 88

Scientists have developed and

tested a new imaging technique

that reveals the atomic structure

of thin films with unprecedented

resolution. For the first time, the

technique has shown very precisely

how the atoms of the first layers of

a film rearrange under the action

of the substrate on which the film

is grown. The results of the study

are reported as the cover story of

the October, 2002 issue of Nature

Materials.

ìThis technique directly provides a

very precise image of atomic positions within a film and at the interface between a film and a substrate,î says Ron Pindak, a physicist at the NSLS and one of the authors of the study. ìWith the current growing interest in the study

of nanomaterials, which are the

size of a few atoms, this technique

will probably be key in devising

such materials and understanding

their properties.î

Thin films are currently used in

many technologies, including electronic chips, coatings, and magnetic recording heads. To improve

the properties of these materials

and create even thinner structures

ñ such as smaller electronic chips

ñ scientists are now trying to understand how the films interact with

the substrate on which they are

grown.

ìWhen you build a film on a substrate, the positions of the atoms

of the film are slightly shifted, and

some of these shifts can be very

small,î says Roy Clarke, a physicist at the University of Michigan

in Ann Arbor and another author

of the study. ìSo it is important to

be able to explain how these films

behave at the atomic level.î

By building upon traditional x-ray

New Technique Reveals Structure of Films With High Resolution

diffraction, the newly devised technique provides such information. In

this technique, x-rays are projected

onto the film and the substrate pattern, which is then used to determine the positions of the atoms inside the film. The diffraction pattern of thin films is composed of

ridge-like features called ìBragg

rods,î hence the name of the technique: coherent Bragg rod analysis (COBRA).

The COBRA technique determines

two key properties of the diffracted

x-ray waves: their intensity and

their phase, which describes the

shift in position between the incident and diffracted x-ray waves.

Though the amplitude is easily determined from the diffraction pattern, the phase is usually more difficult to determine, which is just

what COBRA does.

ìKey to the COBRA technique is a

new approach to determining the

phase of the diffracted x-ray

waves,î says Yizhak Yacoby, physicist at the Hebrew University in

Jerusalem and lead author of the

study. ìUnlike traditional x-ray diffraction techniques, COBRA does

not rely on a priori guesses about

the structure of the film and the

substrate, and we do not need to

prepare the sample in a special way

ñ as with a transmission electron

microscope.î

Yacoby, who started developing the

technique four years ago, first applied it to known structures by using x-rays produced at the NSLS,

which allowed him to refine the

technique. In their recent study,

Yacoby and his collaborators applied the technique to a film made

of gadolinium oxide grown on a

gallium arsenide substrate using

brighter x-rays at the Advanced

Photon Source (APS) at Argonne

National Laboratory in Illinois. Key

to the successful data collection

were two APS beam lines that

Clarke and Edward Stern, a physicist at the University of WashingElectron density map of gadolinium

atoms (located around the peaks) in the

gadolinium oxide film, obtained by

using the COBRA imaging technique.

Ron Pindak Roy Clarke Yizhak Yacoby
2 - 89 Surfaces, Interfaces, and Nanomaterials

ton in Seattle, perfected for the

past five years.

The researchers made unexpected

observations. They noticed that two

thirds of the gadolinium atoms in

the first few layers of the film adjust to match the positions of the

atoms in the substrate. The researchers also discovered that the

structure of the first layers of the

film mimics very closely the

Electron density map of one of the layers of the gadolinium oxide film close to the gallium arsenide substrate (left) and a

layer in the substrate (right), by using the COBRA imaging technique. A comparison of both maps shows that the gadolinium

atoms (around the yellow-red peaks) rearrange so that the maps mimic each other.

substrateís structure, while the atoms in the layers farther away from

the substrate are arranged more

like those in the bulk form of gadolinium oxide. The layer stacking

of the film also appeared to mimic

very closely the substrateís structure.

The scientists now intend to investigate the properties of various

other films. Yacoby, who has already submitted patents for the

COBRA technique, is confident that

it will have many applications in the

design of electronic devices based

on thin films, the self-assembly of

layers made of metal oxides used

in catalysis, and the study of films

made of large organic molecules,

such as proteins.

 -Patrice Pages
Feature Articles 2 - 90

A team of scientists from BNL,

Harvard University, and Bar-Ilan

University in Israel have grown ultrathin films made of organic molecules on the surface of liquid mercury. The results, reported in the

November 15, 2002 issue of Science, reveal a series of new molecular structures that could lead

to novel applications in

nanotechnology, which involves

manipulating materials at the

atomic scale.

Growing molecular films on liquid

surfaces is part of an ongoing activity by Brookhaven scientists to

create nanomaterials, which are a

few billionths of a meter in thickness. Ultrathin films are becoming

increasingly important for fast-developing applications, such as

faster and smaller electronic and

magnetic devices, advanced biotechnological membranes, and controlled drug release in the human

body. The Brookhaven team is a

leader in the field of liquid surfacesupported film growth, with expertise gained over the past 20 years.

ìWhen you grow a film on a solid

surface, the molecules of the film

tend to interlock with those of the

underlying support,î says Benjamin

Ocko, the Brookhaven physicist

who participated in the study. ìBut

an underlying liquid surface is not

ordered and provides an ideal setting for studying ultrathin states of

matter without the complications

of the solid support.î

Ocko and his colleagues first filled

a small tray with liquid mercury and

then deposited on the surface a

nanometer-thin film of stearic acid,

an organic waxlike material that is

a common component of cell membranes. Since stearic acid is not

soluble in mercury, it floats on the

surface.

Molecular Film on Liquid Mercury Reveals New Properties

To see how the molecules of the

film organize on the surface, the

scientists measured how x-rays

produced by the NSLS scattered off

the ultrathin molecular film. Key to the

study was a unique instrument used for tilting the x-rays downward onto the liquid

mercury surface,

which was developed

by Peter Pershan, a

physicist at Harvard

and one of the studyís

authors, along with

the Brookhaven team.

The scientists discovered that, as

the number of molecules deposited

on the surface increased, they

formed four distinct patterns.

ìFirst, when a few molecules are

deposited, they tend to take as

much space as they can, by lying

on the surface,î explains Henning

Kraack, a physics Ph.D. student

This schematic drawing shows how the stearic acid molecules of the film rearrange

as they are added onto the surface of the liquid mercury support.

Ben Ocko

from Bar-Ilan and the studyís lead

author. ìWhen more molecules are

added, a second layer of molecules

lies on top of the first one.

ìThen, as even more

molecules are deposited,î Kraack continues,

ìthey ëstand upí to

leave more space to

neighboring molecules,

allowing them to

densely pack in one

layer. But even then,

before standing up

straight, the molecules

are first tilted to the

side, and stand up completely only

when they are ësqueezedí by other

molecules that ëelbow their way

through.íî

These observations came as a surprise, since previous studies have

shown that, when stearic acid molecules are deposited on water ó

the only other liquid support studIncreasing coverage
2 - 91 Surfaces, Interfaces, and Nanomaterials

ied so far ó they only stand up on

the surface. ìPatterns in which

molecules lie flat on a liquid surface have never been observed

before,î Kraack says.

Moshe Deutsch, a physicist at BarIlan and one of the authors of the

study, notes that because the liquid mercury does not seem to influence too much the way the

stearic acid molecules assemble,

ìgrowing films on a liquid surface

is like growing them without support at all.î It might be possible to

choose a film pattern, he adds, simply by selecting the appropriate

molecular coverage.

ìThis work shows that without an

underlying lattice, we can control

film growth,î Deutsch says. ìBy

growing other molecules on a liquid support, we will be able to control the size and properties of other

films, and thus tailor them for different applications, in particular

their use in nanoelectronics and

nanosensor technology.î

 -Patrice Pages
2 - 93 Surfaces, Interfaces, and Nanomaterial

FUNDING

National Science Foundation (DMR)

Department of Energy (DOE)

PUBLICATION

L. Zhu, et al. ìNanotailored crystalline

morphologies in hexagonal perforated

layers of a self-assembled PS-b-PEO

diblock copolymer,î Macromolecules, 35,

3553 (2002).

FOR MORE INFORMATION

Lei Zhu, Prof. University of Akron, Ohio

lei@polymer.uakron.edu

BEAMLINE

X27C

L. Zhu1, P. Huang1, W.Y. Chen1, Q. Ge1, R.P. Quirk1, S.Z. D. Cheng1, E.L. Thomas2,

B. Lotz3, B.S. Hsiao4, F. Yeh4 and L. Liu4

1

University of Akron; 2Massachusetts Institute of Technology; 3Charles Sadron Institute,

Strasbourg, France; and 4

State University of New York at Stony Brook

Chemicals made of chain molecules called block copolymers can selfassemble into various ordered structures, such as lamellae, cylinders,

and spheres. Using self-assembled crystalline-amorphous block copolymers, scientists have grown ordered polymer nanocrystals, which are

expected to be used in advanced optical applications. X-ray scattering

studies at the NSLS revealed that, simply by varying the crystallization

temperature, the tiny crystals can orient in different directions with respect to the interface between the crystalline and amorphous domains

in the copolymer. Crystal growth can also be tailored in specific directions by conforming to the geometry of the block copolymer nanophases

at high temperature.

Polymers in a confined space of a

few nanometers, or billionths of a

meter, are expected to exhibit a different structure, stability and morphology than ordinary bulk polymers. For instance, the polymers

can be confined in mesoporous inorganic materials, which are made

of pores that are 2 to 50 nanometers in diameter. But if no specific

interactions occur between the inorganic material interfaces and the

crystalline polymers, it is very difficult to drive polymers into the

nanopores.

To avoid this constraint, a team of

scientists from the University of

Akron in Ohio, the Massachusetts Institute of

Technology, the Charles

Sadron Institute in

Strasbourg, France, and

the State University of

New York in Stony Brook

has been successfully

using mesophases (typically ordered phases

with submicron sizes) of

a crystalline-amorphous

diblock copolymer ñ

which form by simultaneous self-assembly

process ñ to study confined polymer crystallization in nanospaces.

The copolymer, called polystyreneb-polyethylene oxide (PS-b-PEO),

is made of polystyrene (PS), an

amorphous polymer with a glass

transition temperature of 100 degrees Celsius, and polyethylene

oxide (PEO), a crystalline polymer

with an equilibrium melting temperature of 69 degrees Celsius.

Because of their distinct chemical

nature, PS and PEO strongly segregate from each other, so after the

PS matrix glassifies, the crystallized

PEO blocks are completely confined

within the nanospaces of the copolymer.

The PEO nanocrystals were investigated on macroscopically-oriented (a single domain in microns

or even milimeters) PS-b-PEO

single crystals using simultaneous

small and wide-angle X-ray scattering (SAXS and WAXS) techniques at the NSLSís Advanced

Polymer beamline X27C. The detailed experimental setup is displayed in Figure 1.

High-resolution SAXS revealed that

the PS-b-PEO sample with 0.39

percent of PEO in volume exhibits

a hexagonally perforated layer

(HPL) phase, where the PS and PEO

layers are alternating and each PEO

layer is made of twodimensionally packed

PS perforations, as

shown in Figure 2.

The researchers also

studied how the

nanolayers and nanoPS cylinders in the PEO

layers affect the crystallization behavior of

the PEO blocks. The

WAXS results showed

that the PEO crystal

orientation in the HPL

phase changes with

the crystallization

Authors (from left): Lei Zhu, Stephen Z.D. Cheng and Ping

Huang.

Tailor-Made Polymer Nanocrystals
Science Highlights 2 - 94

Figure 2. Nano-tailored PEO crystalline

morphologies at (a) -50 °C ≤ Tc≤ -10

°C and (b) Tc ≥ 0 °C. A nanophase is

defined by x, y, and z, and crystal unit

cell axes are a, b, and c. The top view

of the HPL phase is shown at the

bottom, and the side view at the top.

Figure 1. Experimental setup for

simultaneous SAXS and WAXS at

beamline X27C at NSLS.

temperature. At low temperatures,

the PEO crystals preferentially arrange parallel to the layer plane

(Figure 2a top), while above zero

degree Celsius, the crystals become inclined with respect to the

layer plane (Figure 2b top). The

team also noticed that the ribbonlike PEO crystal grows along the

arrays of the hexagonal PS perforations (Figure 2b bottom).

Surprisingly, the WAXS experiments showed that crystal orientation forms in an early stage of

crystallization with a crystallinity of

~ 7 weight percent. The early

stage crystal orientation clearly

reflects the confined effect on polymer crystallization in nanospaces.

These results not only show the

scientistsí ability to manipulate

polymer crystalline morphologies

confined in nanospaces, but also

reveal the details of polymer crystallization on the nanoscale. Further study will investigate the crystal orientation mechanism and explore polymer crystallization in

compounds with more elaborate

mesophases, such as double

gyroids.
 	

	








	


	




	!"# $%

&'!!( " &





	



&#) *!+
,#!-

.#&-$/0
.&-

 12345335







&-# *!!"

 
(! $/6!7


"	

7 


!-89!96!

	

:51* 	

			

			


	


		






/6!7
"	

7 ; 9  $#

7

	






	


 !"






"
"

#$%


"
&'

	(


	


	$


"		
	



		


")
$&

 		
 	 


	
	




 


 	 		

 
 	
 


	



		
	


	


	



	




	

	

	 

	

 









	




 

	 		
 
 	




 


 

	 


	 
	

	


	
 
 
 

 		



	
	





	




	

 



 


	

!  

 	
 

	

	

			
			


	
		

	




	

 

 !! 
 
" 


	

!




	



	
	

		



"	
	

		






	

		


 
  
 





	
	
	



	  
 	






		








#
	



	 




 	

  
	 


	
 


 	
	
  		


	


	





  	  	 	

	 
"

   	
	




   
  
	 




  	 

	


 	 

 		












 
"
 	 




	


	




	
 
 	
 



				




	

	
	





	
"	



 
	



 $%%!



	&'('
	
$)*+

	!

	 

 

	 !	"			
	#$%&				

	"
		"		 '
	"		

"		
	(	
)*
#+%+, -"
)*.	"	!/

	
 0 !
	1
		
			(	
)*"	2 "		


	, "		"	
			$3
	4#56&7%&28-"
)*

		"	4	
94"		
	8 "				"	

	
	


!"		

	::		
	
				


		!! 0	
	
	"0
		;90

;		
	


 $%% 
"


 	



	
	
		





,-.

/0
!  




,)1
	
2


"	
	

		
!	


	
  
 


	 	
 
 ,1 /  




	
 

 	







 
 



"

	
	



	
	



		3





	  	
 	 





 
 

  



	
			




 	 
 		


 


	






	
		



		
	


	 4		4 

	

	

!

 
	 	
	

2 - 97 Surfaces, Interfaces, and Nanomaterial

FUNDING

U.S. Department of Energy

National Science Foundation

PUBLICATION

I. K. Robinson, P. A. Bennett and F. J.

Himpsel, ìStructure of Quantum Wires in

Au/Si(557),î Physical Review Letters, 88,

096104-1 (2002).

FOR MORE INFORMATION

Ian Robinson, Department of Physics,

University of Illinois at Urbana-Champaign

robinson@mrl.uiuc.edu

BEAMLINE

X16A Structures of Quantum Wires in Gold/Silicon(557)

I. Robinson1, P. Bennett2 and F. Himpsel3

1

University of Illinois; 2Arizona State University; and 3University of Wisconsin

Scientists working at NSLS beamline X16A have revealed the full threedimensional structure of nanowires formed by deposition of gold on a

stepped silicon surface using surface X-ray diffraction. The result is important because of the unusual band-dispersion properties previously

reported for this system. The result is interesting because the gold

atoms are neither imaged by STM, nor are involved directly in the electronic states responsible for the metallic behavior of the surface.

A ìquantum wireî is a one-dimensional wire created by arranging

metal atoms that touch each other

in an exact straight line. The wave

functions describing the electrons

present in such a wire are localized in the directions perpendicular to its axis but can form solitons

ñ waves that propagate with little

loss of energy and retain their

shape and speed after colliding

other such waves ñ in the direction along the wire. The Pauli exclusion principle forbids the free

propagation of these solitons along

the wire and leads to a one-dimensional metal with highly unusual

properties.

We have investigated a quantum

wire in a candidate system for spincharge separation, due to the formation of a Luttinger liquid, in

which electrons have long-range

interactions between them.

We used two techniques. The first

is the scanning tunneling microscope (STM), which uses electron

tunneling to map the positions of

individual atoms and defects in a

surface. Typical defects are vacancies, steps and kinks. We also used

surface x-ray diffraction, a traditional structure-determining

method that is less useful for looking at defects, but provides accurate three-dimensional structures.

We measured a large set of crystal

truncation rods to solve a crystalline structure formed by evaporation of 20 percent of a monolayer

of gold onto a silicon(557) surface

using the surface x-ray diffraction

facility at NSLS beamline X16A.

The derived structure, shown in the

figure, reveals four main features.

First, the row of gold atoms sits in

the middle of the terrace between

adjacent steps in the substrate,

while we expected that the metal

would have directly lined the step

edge instead. Second, an almost

ideal substitution takes place in the

upper bilayer, resulting in bond

lengths between gold and silicon

of 2.47 angstrom and 2.35 angstrom, which are indistinguishable

from the bond length between two

silicon atoms, which is 2.35 angstrom. A gold atom appears to substitute in the silicon lattice with

relatively little strain. The third feature is that the step edge reconstructs to form a five-membered

ring, but removes a dangling bond.

Finally, the figure shows a row of

adatoms attached to dangling

bonds.

The STM micrograph reveals two

lines per unit cell that might be

mistaken for wires. The X-ray

structure has only a single gold per

unit cell. Analysis of the inter-row

Peter Bennett (left) and Ian Robinson standing in front of the X16A beam station

at the NSLS.
Science Highlights 2 - 98

distances shows that neither of the

rows can be gold atoms, which are

therefore not visible to STM. The

rows correspond instead to the

(Left) Side view of the three dimensional structure of gold nanowires grown on a silicon(557) surface.

(Right) The STM image shows two rows of atoms, neither of which corresponds to the single gold atom in the

unit cell structure.

step-edge silicon and the adatom

silicon features. Because STM is

surface-sensitive, it detects only

the outermost electron shells of the

topmost layer, whereas surface xray diffraction sees the full threedimensional arrangement of the

atom cores.

7.0Å 7.3Å 5.2Å

7.3±0.7Å
2 - 99 Surfaces, Interfaces, and Nanomaterial

PUBLICATION

T. M. Owens, K. T. Nicholson, M. M.

Banaszak Holl, S. S ̧zer J. Am. Chem. Soc.

124, 6800 (2002).

FOR MORE INFORMATION

Mark M. Banaszak Holl, Associate Prof. of

Chemistry, Univ. of Michigan, Ann Arbor

mbanasza@umich.edu

BEAMLINE

U8B

The physical properties of metal

surfaces can be modified through

the adsorption of small molecules.

For example, hydrocarbons modified with carboxylic acid (RCOOH)

or thiol (RSH) functional groups

have been particularly well studied. In recent years, scientists have

shown that the adsorption of

alkanethiols (CH3(CH2)nSH) on gold

surfaces may have many applications, including molecular electronics and micro-contact printing. But

these applications have met

some limitations due to surface defects introduced by

the adsorption process and to

degradation caused by atmospheric ozone. We have explored the use of alkylsilanes

(CH3(CH2)nSiH3) as a replacement for the thiol groups.

We synthesized monolayers

of hexylsilane (C6H13SiH3),

octylsilane (C8H17SiH3), and

octadecylsilane (C18H37SiH3)

by exposing gold surfaces to

one of the alkylsilanes (Figure 1) in an ultrahigh

vacuum (UHV) chamber. The

gold-alkylsilane samples

have been characterized in

UHV by reflection absorption

infrared spectroscopy

Formation of Alkylsilane-Based Monolayers on

Gold

A team of chemists from the University of Michigan in Ann Arbor have

made a surprising discovery: At room temperature, the chemical reaction of compounds with silicon-hydrogen bonds with gold surfaces yields

a new class of alkylsilane(CH3(CH2)nSi)-based monolayers. The monolayers are reminiscent of the self-assembled monolayers (SAMs) formed

by alkanethiols (CH3(CH2)nSH). However, they exhibit a different chemical behavior that may prove advantageous in microelectronics and micro-contact printing. The alkylsilane monolayers have been characterized using soft X-ray photoelectron spectroscopy (SXPS) and reflection

absorption infrared spectroscopy (RAIRS).

(RAIRS) at the University of Michigan in Ann Arbor, and soft x-ray

photoelectron spectroscopy (SXPS)

at beamline U8B at the NSLS.

The silicon 2p core levels were

measured to have a binding energy

of -99.8 electronvolts (eV), as

shown in Figure 2A, suggesting

that silicon is bound to the gold

surface and that no silicon-hydrogen bonds remain. We measured

a full width at half-maximum of 0.4

eV, which is smaller than that observed for bulk, crystalline silicon

using the same beamline and

monochromator, thus indicating

that silicon atoms are in a chemically homogenous environment.

The valence band spectra of the

alkylsilane-based monolayers (Figure 2) bear a striking resemblance

to valence band data of frozen alkanes (CnH2n+2) of the same length,

indicating that the hexyl, octyl, and

octadecyl chains have remained intact.

We have not observed a silicon-hydrogen stretch in the

RAIRS spectra for alkylsilane

monolayers on gold (Figure

3). The silicon-hydrogen

stretch at 2150 cm-1 is the

most intense feature observed for liquid alkylsilane

(Figure 3D). The absence of

this feature in the monolayers suggests that no siliconhydrogen bonds remain after

chemical adsorption. The observed carbon-hydrogen

stretching modes between

2850 and 3000 cm-1, are consistent with the alkyl (CnH2n+1)

chains being angled away

from the surface.

T.M. Owens1, K.T. Nicholson1, M.M. Banaszak Holl1, and S. S ̧zer2

1

University of Michigan; 2Bilkent University, Ankara, Turkey

Dow Corning Corporation; National

Science Foundation; Fulbright Fellowship

for Sefik S ̧zer; Alfred P. Sloan Fellowship

for M. M. Banaszak Holl; Division of

Materials Sciences and Division of

Chemical Sciences, U.S. Department of

Energy.

FUNDING

Clockwise from top left: Mark Banaszak Holl,Sefik

S ̧zer, Ken Nicholson, and Tom Owens (lead author).
Science Highlights 2 - 100

Figure 1. Schematic representation of alkylsilane (CH3(CH2)nSi) bonding to gold surface.

Figure 3. Reflection-absorption infrared spectroscopy

(RAIRS) spectra (3050-2750 and 2350-2000 cm-1) for

monolayers of (A) octadecylsilane, (B) octylsilane, and (C)

hexylsilane on gold. A solution infrared spectrum of

octylsilane (D) is included for comparison.

Figure 2. X-ray photoemission spectra

(photon energy = 160 eV) of (1)

octadecylsilane, (2) octylsilane, and (3)

hexylsilane monolayers on (4) gold. (A)

Silicon 2p and gold 4f core levels, and

(B) valence band.

Intensity (Arb. Units)

Binding Energy (eV)

Wavenumber (cm-1)

Relative Transmittance

The combination of SXPS and

RAIRS data suggests that when the

alkylsilane monolayers bind to the

gold surface, all three silicon-hydrogen bonds react with the gold

surface and silicon forms bonds to

three surface gold atoms, which is

unlike single gold-sulfur bonds in

structures made of thiol bound to

gold.

Also, the alkanethiol and alkylsilane

layers exhibit different oxidation

behaviors. Oxidation of sulfur atoms causes alkanethiol monolayers to fall apart, while oxidation of

the alkylsilane layers knits the silicon atoms together by forming a

siloxane network and maintaining

the integrity of the alkyl chains and

the surface monolayer.

The unique properties of the

alkylsilane layers may lend them

to applications requiring durable

layers and may provide an interesting route for the formation of

patterned structures.
2 - 101 Surfaces, Interfaces, and Nanomaterial

FUNDING

National Science Foundation

PUBLICATION

B.N. Thomas, R.C. Corcoran, C.L.

Cotant, C.M. Lindemann, J.E. Kirsch, P.J.

Persichini, ìPhosphonate Tubules IIî, J.

Am. Chem. Soc., 124, 1227-1233,

(2002).

FOR MORE INFORMATION

Britt Thomas, Department of Chemistry,

Louisiana State University, Baton Rouge

bthomas@lsu.edu

BEAMLINE

X10A

Scientists are currently studying

how to build novel materials the

size of a few nanometers (a few

billionths of a meter, or the size of

a few atoms), and the conditions

under which these tiny materials

could self-assemble spontaneously

into specific configurations. Understanding the self-assembly process

is one of the most important objectives of nanotechnology, because this process could lead to

materials with completely novel

properties.

Perhaps the most familiar

example of self-assembly

is the formation of vesicles

from phospholipids (lipids

typically found in cellular

plasma membrane)

placed in water. The

vesicles form under the

action of divergent forces

on the phospholipidís long,

water-insoluble (hydrophobic) hydrocarbon tails,

and its compact, watersoluble (hydrophilic)

ìheadgroup.î These divergent forces drive self-assembly. For example, the

hydrophilic headgroups lie

exposed upon the inner

and outer surfaces of

Tubules are stable, hollow, cylindrical crystalline tube-like structures a

few micrometers (millionths of a meter) in size, with potential applications in nanofabrication and medical encapsulation. Stringent control of

the kinetics of the process by which these tubules self-assemble is necessary to control the dimensions and qualities of the tubules. An alternative control mechanism involves subtle chemical modifications made

to the self-assembling molecules. By using x-rays produced at the National Synchrotron Light Source, scientists have studied both control

pathways to understand better how subtle changes made to lecithin, a

molecule found in egg yolks and the plasma membrane of plant and

animal cells, causes rigid, hollow tubules to form.

Phosphonate Tubules

spontaneously formed spherical

vesicles, while their hydrophobic

tails lie sheltered in between the

two hydrated surfaces.

We are now learning that factors

far more subtle than the simple

ìhydrophobicî and ìhydrophilicî

forces can have profound consequences upon the morphology of a

self-assembled material. For example, small, inflexible sections can

be inserted in the phospholipidís

otherwise flexible hydrocarbon tails

by creating triple bonds in the tails.

When this change to the tailís shape

is made, then cooling the resulting

spherical vesicles leads to the creation of rigid, hollow 30-by-0.5

micrometer (millionth of a meter)

vesicles of an astonishing cylindrical symmetry (Figure 1).

Close examination of these cylinders, called tubules, reveals two

unusual features: the tubules are

coaxially nested sets of cylinders,

also called lamellae, and the tubules possess a helical,

hence chiral, substructure.

Tubules form through the

helical winding of a uniform-width phopholipid

bilayer ribbon, which creates a cylinder that serves

as a ìnucleusî for subsequent coaxial windings.

Interestingly, the tubuleís

helical sense of handedness depends upon the

chirality of the tubuleforming molecule: molecules of one chirality produce tubules possessing a

right-handed helical structure, while molecules of

the opposing chirality alB. Thomas1

, R.C. Corcoran2, C. Cotant2, J. E. Kirsch2, C.M. Lindemann3, and P. J.

Persichini4

1

Louisiana State University, Baton Rouge; 2University of Wyoming; Laramie; 3Merck &

Company, Whitehouse Station, New Jersey; 4

Allegheny College, Meadville, Pennsylvania

Authors (clockwise

from left): Phillip

Persichini, Christopher

Lindemann, and Britt

Thomas.
Science Highlights 2 - 102

Figure 2. The tubule-forming 1,2-bis(10,12-

tricosadiynoyl)-sn-glycero-3-phosphocholine.

The arrow indicates the oxygen atom removed

to make the tubule derivative investigated in

this study. The moleculeís chiral center lies

two atoms at the right of that of this oxygen.

Figure 1. Some phosphonate tubules observed with

an optical microscope.

ways produce left-handed helices.

To understand better tubule formation, we have made synthetic perturbations to tubule-forming molecules and characterized the new

products. While it is clear that the

tailsí diynes are required for tubule

formation, the remarkable helical

handedness-molecular chirality

correspondence suggests that by

altering the molecule near its chiral

center, significant changes to tubule morphology could result. Indeed, we have found that removing the phosphoryl oxygen that

links the headgroup to the tails of

the tubule-forming molecule called

1,2-bis(10,12-tricosadiynoyl)-snglycero-3-phosphocholine, we have

doubled the tubule diameter (Figure 2). This change in tubule diameter is significant, since previous studies have succeeded in

changing tubule length, but not its

diameter.

Tubule gross morphology can be

quickly measured by microscopy,

but such measurements are both

static and insensitive to the tubuleís

interior structure. The high intensity of the x-rays produced at beam

line X10A of the NSLS has allowed

us to perform kinetic small-angle

x-ray scattering (SAXS) studies of

the transition between spheres and

tubules. These studies revealed

that: (1) the transition is of the first

order (spheres and tubules are in

equilibrium during the transition)

and is reversible; (2) tubular interlamellar spacing is tightly conserved when tubule diameter is

doubled; and (3) the number of

lamellae is halved when the tubule

diameter doubles. These surprising results about tubule interior

structure give important clues

about intrinsic membrane curvatures and bending moduli, which

are unobtainable by any other

means.

Tubule dimensions and morphology

suggest a host of potential technological applications, ranging from

nanofabrication and purification to

medical encapsulation. Our work is

one step into realizing this technological potential, which will ultimately require optimizing the

tubuleís morphology for a given

application, and understanding not

only its ìgrossî structure but its

interior structure as well.
 	


	


	



	





	






	











	 

	



	
!
"#
$
!%&
#



#&'



	

	())

 )
	
(

	

* 



)


+)
)


	)	
,
-






. /012342245







#&
	





$)
 %


678)

	

19

		


	
	


 	 


 






   	  	
 




	
	



	
 	  
	


  
	



	
	
	







	
	



	
 
 	 
	 !"


 
 
	
	 	 	



	  	 


	 

#
" 
 	
$
	 %& &





"

 %
	
	 	
 	



	






	
	



 
	 	 	
 '


		
$
	


	  	
 








 
	 	
 	 



	
	





#

 ( '
' 


'	
 
 
(	 

 
	
		  

	
	
 
	 ) '


	
 	   '	
 	


(
	


	


	


		


	
	

		

	




   	
   

 




 
!


"
#

 !
" 

 $

"



	





"%




"


"
%
	

&


&
	

"

"




"
	%
	

&


		


$

	

	

'	



#
	


$ #% 
 
(



	
	
	


*+
#
	



,-	




  	  
' 	


  
 	 	 '	







	

.
		



   	 



	 	 
	






	 




/#/ #!#
 /0!- 	

!#!#
 !+0 
'


)
	
	



	
	
	




'	
	
	
(	

  	
 
' 	


	
'

(#%

	)


		   /0!-

	!+0


 	
	


	  	'
	 
 	
  




	

)		


  	 ( 	







	











	
	



	
  
  )

	
'



		


 '	
 
(   

	  	
  	
 


			


(
	



		
)


	

	



'	
	


	
	





			





		






	.	'	


	
 	   
	

 
 #%  

 	

	 
  '	
 
' 

	
	
	

	'
	


	

		

	


				







$)
 
%
:
$)
 
	



*






$)
 
%





 

#% 	  
 




 
	

.	




/0!-	!+0








	
$
		




 123/ 


	4,	
1		




 5 
 6

123/
$


		
	
	

	
	
$




   



	 6	'		




 

   




 		 


 

	   

 


		


	

78

	




	


 

	

	

	


	9
	

) 123/ 

  


 
'	
 	 /0!-



  
 
( #%

	

	
	



	



/0!-



	
	
	


 $ 
	  	



		




	


		'	


 	 *:  . 

	

!+0

			

		


		'

	
	/0!-	


	'$


!+0	
(#%


.	
 
 


	




/0!-	!+0
(

#%.
	




 

	 	
   /0!-




(#%




	

		

	
	


!+0



	
(#%
	
	



	   !+0  


	






	

	


 /0!- 	 	 	
 







	

	/0!-

		

 

  
   

   !   " #




#$$%	


  
 % 	
  
& 



   
  $ 

'()*+$%

 
	 +
   
 &


,, +, !

#$,-

%	
&


.




  
 
 
 
 


 ,.,, +- .&



  
     
 /


$%

3 - 1 Year in Review

Highlights From the March 2002 American Physical Society

The stories below describe five of the more than 50 scientific presentations given by BNL scientists at the

American Physical Society (APS) March meeting in Indianapolis, Indiana.

March 18 - 22, 2002

Meeting

New Spin on High-Temperature

Superconductors

Understanding what holds electron pairs together in

high-temperature (high-Tc

) superconductors is one

of the biggest problems in condensed matter physics, says BNL physicist Peter Johnson, who is searching for the explanation.

Like traditional superconductors, high-Tc

 superconductors can carry electrical current with no resistance, or loss. But high-Tc

 superconductors operate

at temperatures where liquid nitrogen, rather than

expensive liquid helium, can do the cooling. This difference would decrease the cost of and increase potential applications for superconducting materials. But

the first step is to understand the mechanism.

Johnsonís National Synchrotron Light Source (NSLS)

research indicates that electron ìspinî plays an important role. Rather than exchanging vibrations with

the crystal lattice (the mechanism for electron pairing in traditional superconductors), electron pairs in

high-Tc

 materials interact by affecting the spin of atoms in the lattice. Understanding the role of spin has

the potential to revolutionize our thinking about the

transfer of electrical current, Johnson says.

Electron Excitations in High-Temperature

Superconductors

BNL physicist Young-June Kim is studying the collective behavior of electrons in materials closely related

to high-Tc

 superconductors. He uses resonant inelastic x-ray scattering (RIXS), a technique developed at

the NSLS, to understand how electrons are moving

around in the system. By comparing the energy of xrays beamed into a sample and those coming out,

this sensitive technique measures how much energy

is transferred to the electrons in the material.

The absorbed energy can result in a variety of excitations, which can be distinguished by RIXS. Kim is

using the technique to study lanthanium copper oxide, an insulating material, and looking at how the

excitations change as the material is transformed to

a high-Tc

 superconductor by gradually substituting

strontium atoms for lanthanum atoms. With improved

sensitivity, the technique may help reveal the mechanisms behind high-Tc

 superconductivity.

Peter Johnson

Young-June Kim
2002 Activity Report 3 - 2

Material with Unusual Electrical

Properties Holds Up to Scrutiny

An unusual material with an extremely high dielectric constant, which may have applications in highperformance capacitors and miniaturized electronics, first described last July by BNL physicist Christopher Homes has stood up to further scrutiny. The

materialís enormous dielectric constant - a property

that determines itís ability to separate positive and

negative electrical charges, or become polarized - is

apparent even in thin films of the material, which

are the form necessary for applications in microelectronics.

The scientists are now studying how the material

changes as the chemical composition is altered. This

will allow them to separate intrinsic from extrinsic

effects and to zero in on the mechanism responsible

for the large dielectric constant, Homes says.

Giant Nanomolecule Discovered by

Accident

ìGiant nanomoleculesî may sound like an oxymoron, but these relatively large inorganic structures

may provide big benefits for nanoscience, says BNL

physicist Tianbo Liu. Measuring 5.1 billionths of a

meter in diameter and covered with large pores, the

spherical, cagelike molecules may be useful as ìcontainersî for studying chemical reactions at the

nanoscale. The molecules are themselves magnetically active, and can be used to create even stronger

magnetic materials by loading other compounds inside. One possible application: contrast agents in

magnetic resonance imaging (MRI).

Liu and his collaborators discovered the giant

Tianbo Liu

Wolfgang Caliebe and Ron Pindak

Christopher Homes

nanomolecules at the NSLS and using transmission

electron microscopy. The particlesí orderly arrangement tipped the scientists off that they were seeing

something unique: nanoparticles with a uniform size.

Ordinary nanoparticles vary in size. But these particles are molecules, with a definite molecular structure, so they are made the exact same way every

time. Having one-size particles is an advantage when

studying and finding applications for nanoscale properties, which are generally dependent on particle size.

Seeing Hidden Structure in Liquid

Crystals

Liquid crystals, the materials used in laptop computer screen displays, optical networking devices, and

other applications, are composed of rod-shaped mol-
3 - 3 Ye

assistants in the offices of Senators Charles Schumer

(D-NY) and Hillary Rodham Clinton (D-NY), and in

the offices of Congressmen Gary Ackerman (D-NY),

Felix Grucci (R-NY), and Steve Israel (D-NY).

The delegation members, representing the synchrotrons located at Brookhaven, Argonne, and Lawrence

Berkeley National Laboratories, as well as the

ìWe tried to demonstrate as much as w

Capitol Hill policymakers that the light so

vide tangible benefits to industry,î Bare 

particularly stressed the fact that these fac

led to many scientific breakthroughs duri

decades and are now helping scientists 

forefront research, particularly in the life 
3 - 3 Year in 

In an effort to increase the visibility of the NSLS and

that of the three other DOE light sources, the chair

and vice-chair of the NSLS usersí committee, along

with their counterparts from the other light sources,

met with officials on Capitol Hill on April 17 and 18.

ìThe overall aim of these visits was to raise the awareness of the synchrotrons and to lobby for increased

budgets for the Office of Science, and for the physical sciences overall,î says Simon Bare, chair of the

usersí committee of Brookhavenís National Synchrotron Light Source (NSLS), organizer and lead spokesperson of the delegation.

On the first day of the visit, the delegation met with

senior members of the Senate and House Energy &

Water Appropriations Committees, the House Science

Committeeís staff, and key members of the Office of

Management and Budget and the Office of Science

and Technology Policy. Pat Fulton, Science Lobbyist

for Stanford University and Jack Bagley, Battelleís

Vice President for External Affairs, had set up all the

necessary appointments for the six one-hour-long

meetings.

On the second day, Bare and Leemor Joshua-Tor, vicechair of NSLS usersí committee, met with legislative

assistants in the offices of Senators Charles Schumer

(D-NY) and Hillary Rodham Clinton (D-NY), and in

the offices of Congressmen Gary Ackerman (D-NY),

Felix Grucci (R-NY), and Steve Israel (D-NY).

The delegation members, representing the synchrotrons located at Brookhaven, Argonne, and Lawrence

Berkeley National Laboratories, as well as the

Synchrotron Science Highlighted for Capitol Hill Policymake

Stanford Linear Accelerator Center, explai

various scientific contributions of these fac

basic and applied science, the economy, hea

security. The light source representatives al

lighted the critical role played by DOE in fund

entific research at the synchrotron sources, an

for an increase in the FY03 budget for sync

science.

ìWe tried to demonstrate as much as we c

Capitol Hill policymakers that the light sour

vide tangible benefits to industry,î Bare sa

particularly stressed the fact that these facilit

led to many scientific breakthroughs during 

decades and are now helping scientists to 

forefront research, particularly in the life sc

April 17 - 18, 2002
2002 Activity Report 3 - 4

APS Division of Physics and Beams, and it is currently supported by Brookhaven Science Associates,

Southeastern Universities Research Association, and

Universities Research Association.

ìI am honored to receive this award, which is related

to my studies at the Stanford Linear Accelerator Center,î said Podobedov. ìSince I came to BNL in 1999,

Iíve been applying similar techniques to study beam

dynamics at the NSLS rings.î

sured the bunch shape evolution of unstable electron and positron beams at the SLC rings. In his

award-winning thesis, Podobedov was able to show

understanding of the detailed structure of the instability and to identify the mechanism that caused it.

At the NSLS, Podobedov has led a team of NSLS staff

in designing and implementing the digital orbit-feedback system. This system stabilizes electron beam

motion, which in turn results in more stable syn2002 Activity Report 3 - 4

Boris Podobedov of the National Synchrotron Light

Source (NSLS) Department has won the American

Physical Societyís (APS) 2002 Award for Outstanding Doctoral Thesis Research in Beam Physics & Engineering.

The annual award was established in 1990 by the

APS Division of Physics and Beams, and it is currently supported by Brookhaven Science Associates,

Southeastern Universities Research Association, and

Universities Research Association.

ìI am honored to receive this award, which is related

to my studies at the Stanford Linear Accelerator Center,î said Podobedov. ìSince I came to BNL in 1999,

Iíve been applying similar techniques to study beam

dynamics at the NSLS rings.î

NSLSís Podobedov Wins APS Award For Outstanding Thesis

Research

April 21, 2002

The award, which consists of $2,500 and a certificate, was announced at an APS meeting in Albuquerque, New Mexico, on April 21.

Podobedov was cited ìFor an experimental study of

the microwave instability in the Stanford Linear

Collider (SLC) damping rings using a streak camera

to correlate each event to the RF. The development

of this sophisticated technique provides a powerful

tool for the study of non-linear instabilities above

threshold.î

Most storage rings, whether used as light sources or

high-energy physics accelerators such as SLC, require high beam current. When the current is increased, electrons or other types of stored subatomic

particles reach a critical density and various kinds of

instabilities tend to occur, which degrade beam quality.

For example, microwave instability affects internal

bunch structure - the way in which particles are

grouped together in a beam - which is often hard to

measure. Using some novel diagnostics as well as an

instrument called a streak camera, Podobedov measured the bunch shape evolution of unstable electron and positron beams at the SLC rings. In his

award-winning thesis, Podobedov was able to show

understanding of the detailed structure of the instability and to identify the mechanism that caused it.

At the NSLS, Podobedov has led a team of NSLS staff

in designing and implementing the digital orbit-feedback system. This system stabilizes electron beam

motion, which in turn results in more stable synBoris Podobedov
3 - 5 Year in Review

people, newest

equipment, and latest techniques in the field of macromolecular x-ray

crystallography.

Half the students came to observe; the other half

came with their own specimens with the goal of solving the structure of a particular enzyme. About four

structures were solved during the course, and each

of these is likely a publishable result.

Designed and run by Bob Sweet and Denise Kranz of

BNLís Biology Department, the program is funded by

a range of agencies. Key support comes from the

lecting data on

their crystal

samples. There are also plenty of occasions for stimulating conversation over drinks and meals.

ìEveryone, teachers and students alike, finds the

experience absolutely riveting. The 60 hours of data

collection are near chaos on the NSLS floor. But each

of us ends up exhausted but happy, having learned a

little from each of the others,î Sweet said.

 -Karen McNulty Walsh

[Editorís note: Reprinted with permission from the BNL

Bulletin - May 17, 2002.]

Workshop Participants
3 - 5 Year in Review

Brookhavenís offering of RapiData 2002, the fourth

in an annual series of crash courses in x-ray crystallography, was once again a huge success. Forty-eight

students from around the world participated from

April 21 to 26.

More formally titled

ìRapid Data Collection and Structure

Solving at the NSLS:

A Practical Course in

Macromolecular XRay Diffraction Measurement,î the program was developed

by BNLís Biology and

National Synchrotron Light Source

(NSLS) departments

to introduce students to the best

people, newest

equipment, and latest techniques in the field of macromolecular x-ray

crystallography.

Half the students came to observe; the other half

came with their own specimens with the goal of solving the structure of a particular enzyme. About four

structures were solved during the course, and each

of these is likely a publishable result.

Designed and run by Bob Sweet and Denise Kranz of

BNLís Biology Department, the program is funded by

a range of agencies. Key support comes from the

NSLS Annual RapiData Course in X-Ray Crystallography Again

Successful

April 21 - 26, 2002

National Institutes of Health National Center for Research Resources, and significant support from DOEís

Office of Biological and Environmental Research.

The course starts with two days of lectures and tutorials taught by BNL scientists and scientists from industry, academia,

and other national

labs - a total of 38

instructors, tutors,

or helpers, many

of them volunteers.

These mentors

then serve as

hands-on scientific

supervisors when

the students move

to the NSLS beam

lines to begin collecting data on

their crystal

samples. There are also plenty of occasions for stimulating conversation over drinks and meals.

ìEveryone, teachers and students alike, finds the

experience absolutely riveting. The 60 hours of data

collection are near chaos on the NSLS floor. But each

of us ends up exhausted but happy, having learned a

little from each of the others,î Sweet said.

 -Karen McNulty Walsh

[Editorís note: Reprinted with permission from the BNL

Bulletin - May 17, 2002.]

Workshop Participants
2002 Activity Report 3 - 6

A workshop on ìFrontiers in Synchrotron Research

on Soft Matter and Biomaterialsî was held from April

24-27 at the Mary Duke Biddle Estate in Tarrytown,

NY. The workshop was co-organized by John Flanagan

(BNL Biology), Ben Ocko (BNL Physics), and Ron

Pindak (NSLS). Seventy-seven attendees from government, university, and industrial labs met at this

magnificent site overlooking the Hudson River.

The workshop participants related exciting advances

and identified open issues in a number of soft matter

and biomaterials research areas including: phase

transitions in confined geometries and at surfaces,

directed self-assembly of soft matter systems into

functional nano-structures, controlled inorganic

growth in an organic matrix, new behavior in complexes such as those formed by lipids and proteins

or liquid-crystals and polymers, and the dynamics of

protein-folding.

The measurements described in these presentations

were mainly carried out at the NSLS and SSRL synchrotrons. Measurements carried out at the APS and

the ESRF synchrotrons were also presented. The latFrontiers in Synchrotron Research on Soft Matter and

Biomaterials Workshop

April 24 - 27, 2002

ter measurements focused on the application of radiation from high brightness sources to study dynamics such as membrane fluctuations and polymer

reptations.

In order for all the synchrotron facilities to more effectively impact these problems, the participants indicated that faster detectors with energy resolution,

flexible geometry, and wide dynamic range were essential, that barriers needed to be reduced to improve the accessibility of synchrotrons to new users,

that better on-site facilities were required for sample

preparation, and that existing information on mitigating radiation damage needed to be assembled into

a report.

Finally, a glimpse into potential new superconducting undulator insertion devices and energy-recovery

schemes for high-brightness x-ray sources was provided. The interactions between the soft matter and

biomaterials researchers were lively and productive

in nature. A follow-up meeting to track progress and

further encourage cooperative ventures is under consideration. - Ronald Pindak

Workshop Participants
3 - 7 Year in Review

On April 25, over 20 girls and

their parents learned about

some of the scientific programs at the National Synchrotron Light Source (NSLS),

and even performed their own

scientific experiments. The

one-day visit was part of the

national ìTake our Daughters

to Work Day.î

At the NSLS, the girls learned

that light can take many

forms, from microwaves to xrays, and have many applications in electronics, lasers, microscopes, and medicine.

NSLS scientist Lisa Miller offered a tour of

the experimental floor to the girls, who discovered how synchrotron infrared light is

used to study diseases like osteoporosis,

osteoarthritis, and Alzheimerís disease.

NSLS scientist Vivian Stojanoff also showed

the girls how the study of protein crystals is

used to develop new drugs. Later, the girls

toured the Control Room, where Machine Operator Gary Weiner told them how synchrotron light

is made.

The girls also performed their own scientific experiments. By suspending an inflated balloon in the cold

vapor above liquid nitrogen, they discovered that the

air inside of the balloon contracts, and then re-expands when warmed up. In another experiment,

the girls found, much to their surprise, that they could

Take our Daughters to Work Day: Mysteries of Light and

Extreme Cold Uncovered

April 25, 2002
2002 Activity Report 3 - 8

of a one-day plenary session and eight one-day-long

workshops on the latest results achieved at the NSLS

in the physical, biomedical, environmental, and instrumentation sciences.

Speakers included: Steven Dierker, NSLS Chair; Richard Osgood, Associate Laboratory Director for Basic Energy Sciences; Patricia Dehmer, Associate Director of Science for Basic Energy Sciences (BES) at

DOE; Judith Vaitukaitis, Director of the National Center for Research Resources, National Institutes of

Health; and Satoshi Ozaki, Acting Deputy Laboratory Director for Science & Technology. John

Marburger, Presidential Science Adviser and Director

of the Office of Science & Technology Policy, was the

meetingís keynote speaker.

In the plenary session, Ozaki opened the meeting by

welcoming the participants and giving an overview

of the major Laboratory programs. Osgood followed

Among the speakers at the 2002 Annual NSLS Usersí Meeting

were: (from left) Satoshi Ozaki, Richard Osgood, Steven

Dierker, all of BNL;Patricia Dehmer, DOE; Leemor JoshuaTor, Cold Spring Harbor Laboratory, NSLS Usersí Executive

Committee (UEC) Chair-Elect; Simon Bare, UOP-LLC, NSLS

UEC Chair; and John Marburger, Presidential Science Adviser

and Office of Science & Technology Policy Director.
2002 Activity Report 3 - 8

Successful Science, Exciting Plans, Record Attendance Characterize This Yearís Annual NSLS Usersí Meeting

May 20 - 22, 2002

The excellent scientific record of the past year, plans

for upgrades of the NSLS, and projects for new light

source facilities were all hot topics at this yearís National Synchrotron Light Source (NSLS) Annual Usersí Meeting, held at BNL on May 20 to 22.

The meeting, which drew a record attendance of 380

participants coming from all over the world, consisted

of a one-day plenary session and eight one-day-long

workshops on the latest results achieved at the NSLS

in the physical, biomedical, environmental, and instrumentation sciences.

Speakers included: Steven Dierker, NSLS Chair; Richard Osgood, Associate Laboratory Director for Basic Energy Sciences; Patricia Dehmer, Associate Director of Science for Basic Energy Sciences (BES) at

DOE; Judith Vaitukaitis, Director of the National Center for Research Resources, National Institutes of

Health; and Satoshi Ozaki, Acting Deputy Laboratory Director for Science & Technology. John

Marburger, Presidential Science Adviser and Director

of the Office of Science & Technology Policy, was the

meetingís keynote speaker.

In the plenary session, Ozaki opened the meeting by

welcoming the participants and giving an overview

of the major Laboratory programs. Osgood followed

Among the speakers at the 2002 Annual NSLS Usersí Meeting

were: (from left) Satoshi Ozaki, Richard Osgood, Steven

Dierker, all of BNL;Patricia Dehmer, DOE; Leemor JoshuaTor, Cold Spring Harbor Laboratory, NSLS Usersí Executive

Committee (UEC) Chair-Elect; Simon Bare, UOP-LLC, NSLS

UEC Chair; and John Marburger, Presidential Science Adviser

and Office of Science & Technology Policy Director.
3 - 9 Year in Review

with an outline of the re-organization of the material

science effort at BNL and the major initiatives within

the BES directorate, in particular, a proposed BNL

nanoscience center.

U.S. Representative Felix Grucci (R-New York, First

District), who was scheduled to speak at the meeting, was detained in Washington. In a message read

by meeting chair Leemor Joshua-Tor, Cold Spring

Harbor Laboratory, Grucci praised the current and

future scientific programs at the NSLS.

In his keynote address, Marburger said, ìWe are beginning the 21st century with a profound revolution

in science based on capabilities in computing and

instrumentation. These capabilities have achieved an

importance as the foundations of contemporary science that earns them a top priority for support. The

National Synchrotron Light Source is one of the key

representatives of this new instrumentation.î

Dierker highlighted the qualities that make the NSLS

such a successful facility. ìWith more than 2,500 scientists from over 400 institutions per year coming

from academic, industrial, and government institutions, the NSLS is a widely used facility,î he said.

ìNot only do we have a large contingent of users,

but also, last year, the users produced more than

800 publications based on research performed at the

NSLS, 150 of which appeared in premiere science

journals.î

In terms of budget, Dierker announced that DOE had

recently added $600,000 to the NSLS budget for

FY02. An additional $1.6 million is also contained in

the Presidentís FY03 budget request. ìAltogether, we

are looking at an increase of $2.2 million next year,î

Dierker said. ìWe are very grateful to DOE and Congress, and we are excited about the opportunities

that this additional funding will allow.î

Usersí Executive Committee Chair Simon Bare (right), UOP,

LLC, presents a photo of the NSLS to Office of Science &

Technology Policy Director John Marburger.

Lonny Berman, BNL, Leemor Joshua-Tor, Cold Spring Harbor

Laboratory; Steven Dierker, BNL, Simon Bare, UOP-LLC.

The 2002 Annual NSLS Usersí Meeting Organizing Committee includes:(from left)

Lisa Miller, BNL; Mary Ann Corwin, BNL; Caroline Kisker, BNL; Nancye Wright,

BNL; Dan Fischer, National Institute of Standards & Technology; Lydia Rogers,

BNL; Leemor Joshua-Tor, Cold Spring Harbor Laboratory; Lonny Berman, BNL;

Anatoly Frenkel, Yeshiva University.

Patricia Dehmer, Associate

Director of Science, Office of

Basic Energy Sciences, DOE.
2002 Activity Report 3 - 10

Dierker also discussed some changes under way at

the NSLS that will improve support for current and

future users. One major change has been an administrative reorganization, to provide better coordination for project management and to place greater

emphasis on support for user science. ìWe expect

these changes to increase productivity and to enable

our users to obtain better research results,î he said.

In announcing longer-term plans, Dierker first hailed

a recent achievement by one of the near-term future

light sources, the deep ultraviolet free electron laser

(DUV-FEL). Last February, the DUV-FEL generated

light at 400 nanometers (billionths of a meter) by a

process called self-amplified spontaneous emission

process.

By fall, Dierker added, the DUV-FEL is expected to

provide radiation at 88 nanometers, to be used in

pioneering chemistry experiments. To advance beApproximately 40 of the 55 posters at

the NSLS Annual Usersí Meeting poster

session, organized by Lisa Miller (NSLS)

were the work of students and postdocs.

yond current NSLS performance by increasing beam

brightness while reducing pulse length, Dierker announced plans for a new facility, which would benefit

from two technological approaches.

One, based on an ultra-low emittance storage ring,

would provide about a factor of 10,000 increase in

brightness. The other, called Photoinjected Energy

Recovery Linac (PERL), would produce high brightness and very short pulse lengths.

ìThe design would start with an ultra-low emittance

storage ring and evolve toward a PERL approach as

that technology develops,î Dierker said. The new facility would be located adjacent to the x-ray ring.

During her presentation on the current programs

managed by DOE-BES, Dehmer was enthusiastic

about the current and future projects at the NSLS.

ìSteve Dierker has done a tremendous job over the

(From left:) Mark Chance, Albert Einstein College of

Medicine; Judith Vaitukaitis, Director, National Center for

Research Resources, National Institutes of Health; Patricia

Dehmer, DOE; and Richard Osgood, BNL.

(From left:) Stefan Kycia, LNLS, Campinas, Brazil; Cam

Hubbard, Oak Ridge National Laboratory; and Peter

Stephens, Stony Brook University.
3 - 11 Year in Review

past year in rethinking the challenges that face

the NSLS,î she said.

Another new project discussed at the meeting

was a center dedicated to the study of the infinitesimally small. Called the Center for Functional Nanomaterials, or Nanocenter for short,

this new BNL facility has received a ìvery strong

thumbs upî from initial reviews by DOE-BES,

according to Ozaki.

The Nanocenter will be organized similarly to

the NSLS, including laboratory clusters, user

and visitor laboratories, and training and seminar facilities, and is expected to be built close

to the NSLS and the Instrumentation Division.

ìThe NSLS and the Nanocenter will be portals to each

other,î said Osgood, who masterminded the

Nanocenter project. ìWe envision both of these facilities as helping each other maintain a strong and

vigorous user base.î

ìBrookhavenís Nanocenter will be a bold departure

from business as usual in the research communities

of materials sciences and chemistry,î Dehmer commented. ìWe are trying to change the face of small

science by locating a lot of disciplines in one place,

so that, if scientists want to pursue a research program that mixes chemistry, biology and materials

science, then they can do it.î

Marburger, in his keynote address, outlined some of

the new changes facing science in the 21st century.

ìScientists are opening the doors to a new kind of

science,î Marburger said. ìNever before had we been

able to relate properties of large-scale matter and

Hiroshi Takahashi (left), BNL, and Rick Bradanick, VAT Inc. (From left:) Janos Kirz, Stony Brook University; Thomas

Vogt, BNL; Richard Osgood, BNL; and Peter Paul, BNL

Interim Director.

big things made of atoms to the detailed atomic structure. Now, we can, and the prospects are truly exhilarating.

ìI look forward to seeing what comes out of this Laboratory, as well as others that I fully expect society to

continue to support,î he added.

During the workshops and part of the plenary session, scientists presented current research and future light source projects. They addressed topics as

diverse as the use of synchrotrons in the environmental sciences, the study of ultra-fast processes with xrays, nanoscale materials, membrane protein crystallography, catalysis, materials processing, synchrotron micro-spectroscopy and imaging, and the development of more advanced light source detectors.

 ó Patrice Pages

Lunch under the ìbig topî next to Berkner Hall on Tuesday, May 21.

[Editorís note: Reprinted with permission from the BNL Bulletin - June 14, 2002.]
2002 Activity Report 3 - 12

Congratulations go out to Gary Nintzel, a member of

the NSLS User Science Division Technical Specialists

staff. Gary is the first recipient of the NSLS Usersí

Executive Committee (UEC) Community Service

Award. This award is for service, innovation and dedication to users of the NSLS.

Gary was nominated for this award by members of

the NSLS user community. Many of the comments

on the nomination form speak volumes for his contributions over the years:

ï ìGaryís support has made the difference between

survival and defeat for several PRTs.î

ï ìWith his extensive knowledge of nearly all the

beamlines on the VUV floor, he is able to diagnose

problems very efficiently, minimizing lost beamtime.î

ï ìIn addition to his regular and untiring support

for the growing number of beamlines under the control of the NSLS User Science Division, he has made

time to provide significant support to nearly all the

other beamlines on the VUV floor, plus X1 and X13.î

Simon Bare, Chair of the NSLS UEC, presented the

award to Gary at the NSLS Usersí Meeting banquet

on the evening of May 21. Gary received a $250 gift

certificate and his name was engraved on a plaque

that is displayed in the atrium of the NSLS.

UEC Community Service Award Presented to Gary Nintzel

May 21, 2002

Gary Nintzel (right), NSLS, is the first

winner of the NSLS Usersí Executive

Committee (UEC) Community Service

Award for service, innovation, and

dedication to users of the NSLS. Nintzel

was presented a with $250 gift certificate

by Simon Bare, UEC Chair, at the Usersí

Meeting banquet on Tuesday, May 21, and

his name was engraved on a plaque that

is displayed in the NSLS atrium.

Gary Nintzel working on beamline U5UA.

 - Simon Bare
3 - 13 Year in Review

A workshop on applications of synchrotron radiation

in the environmental sciences has become a tradition at the NSLS Usersí Meeting.

Two talks on soft X-ray applications were presented:

Physicist Juergen Thieme, of the University of Georgia Augusta in Gˆttingen, Germany, outlined soft Xray spectro-microscopy in studies of geochemical and

environmental processes, and geoscientist Satish

Myneni, of Princeton University, described the structure of water in controlling environmental processes.

Two talks were given on powder diffraction. Jeffery

Post, the Curator of the National Gem and Mineral

Collection of the Smithsonian Institution in Washington, DC, demonstrated his joy in basic research by

discussing real-time powder diffraction studies of the

dehydration behaviors of clays. Geoscientist Peter

Heaney, of Pennsylvania State University in University Park, showed how real time powder diffraction

studies of hydrotalcites could elucidate the mechanism of rapid cation exchange in this class of clay

minerals.

Chemist Hoi-Ying Holman, of Lawrence Berkeley National Laboratory, introduced the possibilities for synchrotron radiation FTIR spectro-microscopy to study

microbial degradation of poly-aromatic hydrocarbon

on mineral surfaces.

Environmental engineer Lisa Axe, of the New Jersey

Institute of Technology in Newark, explained metal

The Environmental Sciences: Synchrotrons Providing Powerful

May 20, 2002

sorption on amorphous iron and manganese oxides

by X-ray Absorption Spectroscopy.

Chemist Martine Duff, of the Savannah River Technology Center in South Carolina, discussed applications of hard X-ray spectroscopy to the field of highlevel radioactive waste treatment and characterization.

BNL geochemist Mark Fuhrmann outlined the applications of synchrotron techniques to

phytoremediation.

The workshop concluded with a roundtable discussion on environmental science at NSLS: Chi Chang

Kao, Associate Chair of NSLS, outlined the NSLS perspective and support for environmental research;

Geoscientist Rich Reeder, of the State University of

New York in Stony Brook, and environmental scientist Paul Kalb, of BNL, outlined the EnviroSuite initiative; BNL environmental scientist Keith Jones discussed the laboratory for Synchrotron-Based Earth

and Environmental Research currently located at

X26A and X27A; Steve Sutton, director of Consortium for Advanced Radiation Sources (CARS) - which

goal is to develop X-ray beamlines at the Advanced

Photon Source at Argonne National Laboratory - outlined the concept for EnviroSync to define needs of

environmental science to synchrotron users.

 -Douglas Hunter

Tools for a New Science Workshop

Workshop Participants
2002 Activity Report 3 - 14

Many regions of the electromagnetic spectrum have

provided critical information on the structure and

dynamics of matter, but x-rays have been especially

useful because their wavelengths are similar to atomic

dimensions. So, x-rays have proven indispensable in

determining the structure of materials at the atomic

level.

In addition to a materialís structure, scientists can

also look at the dynamics of atoms inside the material. Over the past several decades, physicists have

learned how to produce short pulses of light, which

have provided valuable insights into the motions of

various forms of matter, including biological systems.

This workshop focused on the use of ìX-ray Sources

for Studies of Ultrafast Processes.î

Lasers have played a key role in producing short

pulses of visible, ultraviolet and infrared radiation.

These pulses can last between a few billionths of a

second (nanoseconds) to a few billionths of a billionth of a second (attoseconds). Using various combinations of laser and accelerator technologies, scientists are now on the verge of conducting studies of

ultrafast processes at the atomic level using pulsed

x-rays.

The most direct means of generating ultrashort pulses

of x-rays is to focus a laser with a corresponding

temporal structure onto a target, hence generating

a plasma that emits a flash of x-rays. Chemist

Christoph Rose-Petruck, of Brown University in Providence, Rhode Island, described such a system developed in his laboratory for the study of chemical

processes. This system is relatively inexpensive, costing only about half a million dollars and offers all of

the advantages of having a dedicated system.

Two speakers at the workshop described the generation of ultrafast X-ray pulses by Thompson scattering of a laser pulse off relativistic electrons generated by a linear accelerator. Physicist Gwyn Williams,

of the Thomas Jefferson National Accelerator Facility

(TJNAF) in Newport News, Virginia, described experiments performed at TJNAFís Free Electron Laser. BNL

physicist Igor Pogorelsky described the generation

of short X-ray pulses at BNLís Accelerator Test Facility.

Beyond the available or nearly available approaches

outlined above, three speakers described accelerator based X-ray sources in various stages of development that offer the prospects of far greater brightness. Physicist John Arthur, of Stanford Linear Accelerator Facility (SLAC), described plans for SLACís SubPicosecond Pulsed Source (SPPS), which will use that

portion of the SLAC linac not required in the B-factory experiment.

The planned successor to the SPPS at SLAC is the

Linac Coherent Light Source (LCLS), which was described by physicist Stephen Milton, of the Advanced

X-Ray Sources for Studies of Ultrafast Processes Workshop

May 20, 2002

Workshop Speakers (from left):

Christoph Rose-Petruck, (Brown

University in Providence, Rhode

Island), John Arthur, of Stanford

Linear Accelerator Facility (SLAC),

Stephen Milton, (Advanced Photon

Source (APS) at Argonne National

Laboratory), John Sutherland (BNL,

Biology), Joel Brock, (Cornell

University in Ithaca, New York), and

Gwyn Williams (Thomas Jefferson

National Laboratory).
3 - 15 Year in Review

Physicist Scott Calvin, of NRL, chemist Josef Hormes,

the director of the Center for Advanced Microstructures and Devices (CAMD), a synchrotron radiation

research center at Louisiana State University in Baton Rouge, and chemist Robert Schloegl, of FritzHaber-Institute in Berlin, Germany, addressed the

difficulties of quantitatively describing freestanding

nanoparticles.

Physicist Anatoly Frenkel, of Yeshiva University in New

York, made a presentation on nanoparticles embedded within a common amorphous host. Physicist Maria

Grazia Proietti, of the University of Zaragoza in Spain,

and environmental scientist Ken Kemner, of Argonne

National Laboratory, presented their progress in the

study of semiconductor quantum wires and

to allow rapid fitting of unknown atomic structures.

Calvinís work includes the multi-edge fitting of mixed

spinel ferrites and the passivation of metallic iron in

multi-shelled nanoparticles. Calvin is particularly interested in the stabilization of high magnetic moment particles for applications ranging from high frequency electronics to magnetic targeted drug delivery. He described his nanoparticles as having multiple layers of amorphous metal and oxide surrounding a close packed Fe core.

In contrast, Hormes relied heavily upon XANES spectra to establish that the local structure of

nanoparticles are indeed quite different from their

bulk counterparts and that XANES spectra can be

used to track the evolution of valency as the particle
3 - 15 Year in Review

Motivated by the recent excitement of scientists in

the field of nanoscience, which is the study of materials at a scale of a few billionths of a meter, physicist

Vincent Harris of the Naval Research Laboratory (NRL)

in Washington, DC, organized a workshop titled: ìExtended X-ray Absorption Fine Structure (EXAFS) Studies of Nanoscale and Nanostructured Materials.î

Although the workshop was tightly focused on the

use of EXAFS to probe the nanostructure of materials, international speakers also covered magnetism,

biology, geochemistry, catalysis, and electronics.

Physicist Scott Calvin, of NRL, chemist Josef Hormes,

the director of the Center for Advanced Microstructures and Devices (CAMD), a synchrotron radiation

research center at Louisiana State University in Baton Rouge, and chemist Robert Schloegl, of FritzHaber-Institute in Berlin, Germany, addressed the

difficulties of quantitatively describing freestanding

nanoparticles.

Physicist Anatoly Frenkel, of Yeshiva University in New

York, made a presentation on nanoparticles embedded within a common amorphous host. Physicist Maria

Grazia Proietti, of the University of Zaragoza in Spain,

and environmental scientist Ken Kemner, of Argonne

National Laboratory, presented their progress in the

study of semiconductor quantum wires and

EXAFS Studies of Nanoscale and Nanostructured Materials

May 20, 2003

nanoparticles formed via biogeochemical interactions,

respectively.

Calvin and Hormes both presented talks focused on

the use of EXAFS, specifically the use of FEFF-generated theoretical data together with FEFFIT fitting

codes, to describe the local element-specific structure of nanoparticles and core shell nanoparticles.

FEFF is a computer program created at the University of Washington that generates x-ray absorption

fine structure spectra for clusters of atoms. This data

is used by another computer program called FEFFIT

to allow rapid fitting of unknown atomic structures.

Calvinís work includes the multi-edge fitting of mixed

spinel ferrites and the passivation of metallic iron in

multi-shelled nanoparticles. Calvin is particularly interested in the stabilization of high magnetic moment particles for applications ranging from high frequency electronics to magnetic targeted drug delivery. He described his nanoparticles as having multiple layers of amorphous metal and oxide surrounding a close packed Fe core.

In contrast, Hormes relied heavily upon XANES spectra to establish that the local structure of

nanoparticles are indeed quite different from their

bulk counterparts and that XANES spectra can be

used to track the evolution of valency as the particle

Workshop
2002 Activity Report 3 - 16

size is increased during processing.

Schloegl presented a review of his work in the use of

in-situ time resolved EXAFS to understand the local

structure fingerprinting of the phase transformations

of molybdates; a class of materials that hold potential for catalytic applications.

Proietti described the use of Grazing Incidence Diffraction Anomalous Fine Structure (GI-DAFS) to reveal the role of phosphorous in InAs/InP self assembled quantum wires. This talk was a balance of

high quality semiconductor materials processing and

extremely difficult techniques that left the audience

thoroughly impressed.

Finally, Kemner showed the value of the APS as a

state-of-the-technology synchrotron capable of probing the dynamics of ground water contamination in

the burgeoning field of biogeochemistry.

Each speaker generated excitement and active question-and-answer periods that often spilled out into

the corridors. Materials scientist Joseph Woicik, of

the National Institute of Standards and Technology

(NIST) reminded the attendees of the value and importance of presenting raw data for inspection by

the audience.

In summary, the key findings of the workshop were

that EXAFS is a near-ideal tool for the characterization of nanoscale systems, but that it is best used

with other techniques to provide scientists with a

clearer picture of the material under study.

 -Vincent Harris

Workshop Participants

Integral membrane proteins perform some of the

most important functions of living cells, yet understanding their molecular mechanisms through structural studies presents unique challenges. The aim of

the workshop entitled ìPractical Aspects of Membrane

Protein Crystallography: From Overexpression to

Crystallizationî was to discuss the nuts-and-bolts of

over-expressing, purifying, and crystallizing memPractical Aspects of Membrane Protein Crystallography: From

May 20, 2002

brane proteins for structural studies by x-ray crystallography.

Biologist Susan Buchanan, of the National Institute

of Diabetes and Digestive and Kidney Diseases

(NIDDK) at the National Institute of Health (NIH),

made a presentation on the production, purification,

and characterization of bacterial outer membrane proOverexpression to Crystallization Workshop
2002 Activity Report 3 - 16

Integral membrane proteins perform some of the

most important functions of living cells, yet understanding their molecular mechanisms through structural studies presents unique challenges. The aim of

the workshop entitled ìPractical Aspects of Membrane

Protein Crystallography: From Overexpression to

Crystallizationî was to discuss the nuts-and-bolts of

over-expressing, purifying, and crystallizing memPractical Aspects of Membrane Protein Crystallography: From

May 20, 2002

brane proteins for structural studies by x-ray crystallography.

Biologist Susan Buchanan, of the National Institute

of Diabetes and Digestive and Kidney Diseases

(NIDDK) at the National Institute of Health (NIH),

made a presentation on the production, purification,

and characterization of bacterial outer membrane proOverexpression to Crystallization Workshop
3 - 17 Year in Review

teins both refolded from inclusion bodies and also as

membrane-inserted functional proteins.

Cell biologist Da Neng Wang, of New York University,

described the production of bacterial inner membrane

transporters as functional, affinity-tagged proteins,

and methods for optimization of each step in their

production and purification.

Biologist Martine Cadene, of Rockefeller University

in New York, explained the use of the Matrix Assisted

Laser Desorption Ionization (MALDI) mass spectrometry in defining the covalent state of purified membrane proteins, and using this information as an aid

in designing mutant constructs specifically amenable

to crystallographic analysis.

Biologist Miro Venturi, of NIH, described methods for

the production and screening of monoclonal antibodies specifically reactive against the folded conformations of integral membrane proteins. He described

recombinant methods for production and purification

of Fab and Fv fragments of these antibodies, and

their use as crystallization reagents, giving work with

the transporter protein NhaA as a specific example.

Structural biologist Reinhard Grisshammer, of NIH,

ìExpression and Purification of G-Protein-Coupled

Receptors (GPCRs) for Structure Determinationî, gave

a detailed presentation on the expression and purification of functional G-protein coupled receptors as

fusion proteins in E. coli. He gave examples of success with this approach for several different GPCRs.

Barry Springer, director of Molecular Biology and Protein Biochemistry and project team leader at 3-Dimensional Pharmaceuticals Inc. (3DP), presented the

expression of functional GPCRs in mammalian (HEK293) cells, and biophysical and fluorimetric highthroughput assays to assess their functionality and

stability in detergent-containing solutions.

Biophysicist Ehud Landau, University of Texas Medical Branch in Galveston, described the use of cubic

lipidic matrices as a medium for the stable incorporation of integral membrane proteins, and their crystallization in this medium. He presented many examples of highly diffracting crystals obtained using

this methodology.

BNL biologist Dax Fu described the stabilization of

solubilized bacterial transporters by inclusion of their

cognate binding ligands, a necessary precursor to

their successful crystallization.

Biochemist Patrick Loll, of Drexel University in Philadelphia, presented a rational approach to the design

of crystallization screens for membrane proteins,

based on the ìcloud pointsî of detergents in different protein-precipitating conditions. Based on this

approach, he has developed screens containing over

600 potentially useful conditions, near detergent

phase transitions, and demonstrated a high rate of

success with this screen.

 -Larry Shapiro and Filippo Mancia

Workshop Participants
2002 Activity Report 3 - 18

In a successful and informative workshop titled ìRecent Advances in the Application of Synchrotron Radiation to Catalysis,î topics ranged from new developments of using soft x-rays at high pressures to in

situ X-Ray Diffraction (XRD) studies.

Chemist Gary Haller, of Yale University, began the

workshop with a talk on a detailed characterization

of platinum and tin in PtSn-MCM41 catalysts.

Simon Bare, from UOP LLC - a leading company in

developing and commercializing technology for license to the oil refining, petrochemical and gas processing industries, headquartered in Des Plaines, Illinois - showed how theoretical calculations combined

with in situ X-ray Absorption Near-Edge Structure

(XANES) is a powerful combination that provided detailed insight into the chemistry of small platinum

clusters.

Chemical engineer Enrique Iglesia, from the University of California, Berkeley, showed several examples

highlighting both the power and also the drawbacks

of X-ray Absorption Fine Structure (XAFS) in catalyst

characterization, particularly in supported metal oxide catalysts. He emphasized the need that the characterization must be combined with catalyst activity

in order to ensure that meaningful structure-activity

relationships are developed.

BNL chemist Jon Hanson highlighted the applicability of in situ X-Ray Diffraction (XRD) for following

structural phase transformation in bulk catalysts.

The applicability of Near-Edge X-ray Absorption Fine

Structure (NEXAFS) to characterize the electronic

structure of both model and real catalysts was demonstrated by Jingguang Chen, of the University of

Delaware in Newark.

Chemist Robert Schloegl, of

Fritz-Haber-Institute in Berlin, Germany, updated the

workshop on recent developments in using soft x-rays at

more realistic reaction conditions to probe the electronic

structure and chemical form

of the surfaces of working

catalysts. He showed two examples where the activity of

the catalyst was linked to a

particular species that was

only present under reaction

conditions, this highlighting

the need for in situ surface

sensitive spectroscopy.

Chemical engineer and materials scientist Daniel

Resasco, of the University of Oklahoma in Tulsa,

talked about a novel catalyst used for producing

single-walled carbon nanotubes, and how Extended

X-ray Absorption Fine Structure (EXAFS) was critical

in developing an understanding the structure of the

active form of the catalyst.

John Gland, of the University of Michigan in Ann Arbor, used in situ Fluorescence Yield Near Edge Spectroscopy (FYNES) to not only characterize the intermediates present during the total oxidation of hydrocarbons on single crystals of platinum but also to

follow the kinetics of the oxidation.

BNL chemist Jan Hrbek closed out the workshop with

a talk on the use of high resolution X-ray Photoelectron Spectroscopy (XPS), combined with Density

Functional Theory (DFT) calculations, to follow the

sulfidation of a titanium dioxide single crystal surface. -Simon Bare

Recent Advances in the Application of Synchrotron Radiation to

Catalysis Workshop

May 22, 2002

Workshop Participants
3 - 19 Year in Review

Workshop Participants

One of the most well attended workshops at the meeting was entitled ìCombining Synchrotron X-Ray and

Infrared Imaging and Microspectroscopy.î

The goal of the workshop was to introduce and describe the many micro-spectroscopy and imaging

techniques available at the NSLS, including infrared

(IR) micro-spectroscopy, hard x-ray microprobe,

Scanning Transmission X-ray Microscopy (STXM), xray micro-diffraction, diffraction-enhanced imaging

(DEI), and x-ray micro-tomography. The workshop

provided unique insight into why the NSLS is so well

suited for these techniques.

The synchrotron light produced at the NSLS is 1,000

to 10,000 times more intense than that produced at

conventional laboratory sources. The light is also very

highly collimated and covers a broad spectra range,

from x-ray wavelengths as small as 0.1 angstrom to

the far-infrared, with wavelengths longer than 107

angstrom.

These characteristics mean that smaller, more intense beams can be produced, giving scientists the

capability to produce images of extremely small or

dilute samples, determine elemental or molecular

concentration gradients, and probe the chemical

states of elements and compounds in a variety of

materials with very high spatial resolution.

The workshop gave the attending NSLS users a practical sense of the individual techniques available to

them and specific examples of how such techniques

are being used and combined by users to solve complex scientific problems in a variety of fields.

During the morning session, six speakers described

the ins and outs of each technique.

Geochemist Antonio Lanzirotti, from the University

of Chicago, presented a discussion of the X26A

beamline hard x-ray microprobe. With an emphasis

on Earth and Environmental Sciences, X26A allows

users to quantify elemental abundances of materials

in situ with detection limits often better than one

part per million (ppm) and at a spatial resolution of

10 micrometers or better.

Physical chemist Jean Jordan-Sweet, from the IBM

Research Divisionís Thomas J. Watson Research Center in Yorktown Heights in New York, introduced the

attendees to the uses of micro-diffraction imaging at

the X20 beamlines, showing how these instruments

can be used to study interfacial strain caused by residual stresses in materials and for real-time characterization of electro-migration effects with a spatial

resolution as small as 2 μm.

Physicist Chris Jacobsen, from the State University

Combining Synchrotron Infrared and X-Ray Micro-Spectroscopy

and Imaging Workshop

May 22, 2002
2002 Activity Report 3 - 20

A workshop titled ìIn situ studies of materials processingî included speakers using synchrotron-based

x-ray techniques to study materials processes and

speakers outside the synchrotron community.

In situ Studies of Materials Processing Workshop

May 22, 2002

Physicist Randy Headrick, of the University of Vermont in Burlington, kicked off the workshop with an

overview of in situ studies of materials processing.

He outlined the information that can be obtained with

phy (XMT) and how such studies are conducted at

beamline X2B. With image resolutions approaching

1 μm, XMT analysis of medical, industrial, and earth

materials gives users the ability to image the internal structure of macroscopic objects without having

to physically dissect the object.

NSLS physicist Zhong Zhong highlighted the recent

and dramatic advances in Diffraction-Enhanced Imaging (DEI) at the X15A beamline. DEI dramatically

enhances the ability to image and contrast soft tissue in ways not currently possible using techniques

such as Magnetic Resonance Imaging (MRI) and Computed Tomography (CT) imaging. In the field of clinical imaging, particularly with respect to mammography, itís clear that DEI can provide remarkable sensitivity compared to standard radiographic techniques.

NSLS chemist Lisa Miller gave an informative presentation illustrating most effectively how the 500-

1000 times greater brightness of the infrared (IR)

source on the VUV-IR ring in comparison to standard

laboratory sources allows IR studies, often using commercial infrared microscopes, to be done with smaller

spot sizes and higher throughput. Miller showed that

these improvements allow for better resolution of

chemical components in a wide range of materials,

including plant and animal tissue, polymers and laminates, and geological samples.

The six speakers of the afternoon session focused on

various applications, emphasizing the complemen

micro-spectroscopy and micro-diffraction techniques.

Physicist George Flynn, of the State University of New

York in Plattsburgh, provided insight into the elemental mapping of interplanetary dust particles that he

obtained by using hard and soft x-ray micro-spectroscopy, FTIR, and XMT techniques.

Geophysicist Russell Hemley, of the Carnegie Institute in Washington, DC, presented studies of highpressure materials and compounds using FTIR and

x-ray micro-diffraction techniques.

Physicist Marco Di Michiel, of the European Synchrotron Radiation Facility (ESRF) in Grenoble, France,

presented results of a study of fast high-energy xray tomography and site preferences for metal uptake in minerals, using hard x-ray micro-spectroscopy.

Geologist Richard Reeder, of the State University of

New York at Stony Brook, presented his latest results on site preferences for metal uptake in minerals, obtained using hard x-ray micro-spectroscopy.

A ìGuidebook of Micro-spectroscopy and Imaging

Techniques at the NSLSî was distributed to the attendees at the end of the workshop and can be downloaded online at:

http://nslsweb.nsls.bnl.gov/nsls/pubs/nslspubs/imaging0502/imaging0502.htm

 -Lisa Miller and Antonio Lanzirotti
2002 Activity Report 3 - 20

A workshop titled ìIn situ studies of materials processingî included speakers using synchrotron-based

x-ray techniques to study materials processes and

speakers outside the synchrotron community.

In situ Studies of Materials Processing Workshop

May 22, 2002

Physicist Randy Headrick, of the University of Vermont in Burlington, kicked off the workshop with an

overview of in situ studies of materials processing.

He outlined the information that can be obtained with
3 - 21 Year in Review

different synchrotron-based surface x-ray techniques

and assessed the potential of X21 for such studies in

the future.

Physicist Christian Lavoie, from the IBM Research

Divisionís Thomas J. Watson Research Center in

Yorktown Heights in New York, showed how the use

of real-time synchrotron light can dramatically reduce the time necessary to investigate the physical

properties and transformations in a wide range of

cobalt alloy silicides.

Materials scientist Kit Umbach, of Cornell University

in Ithaca, New York, showed how Grazing-Incidence

Small-Angle X-ray Scattering (GISAXS) had enabled

him to follow carefully the formation of ripple patterns on silicon dioxide during sputter erosion with

argon ion beams. His results suggest that the finite

viscosity of the surface plays an important role in

determining the surface morphology.

This work contrasted with that of materials scientist

George Malliaras, of Cornell University, who is developing pentacene-based optoelectronic materials. His

initial Atomic Force Microscopy (AFM) and x-ray scattering results with Headrick suggest that there is an

unusual structure in the first layer of pentacene deposited onto silicon, and that 3-d crystallites nucleate on top of that layer. One of the most powerful

surface x-ray techniques is surface crystallography,

but its effective utilization requires solving the wellknown phase problem.

Physicist Paul Lyman, of the University of Wisconsin

in Milwaukee, showed that, to some extent, this problem could be overcome by using maximum entropy

methods.

The last three talks dealt with very important materials processes for which real-time x-ray scattering

may be able to provide vital information.

Physicist R.D. Vispute, of the University of Maryland

in College Park, discussed the extensive Pulsed-Laser Deposition (PLD) growth efforts at the University

of Maryland, focusing particularly on efforts to develop aluminum nitride dielectric layers for use on

silicon carbide-based devices and to develop widebandgap semiconducting zinc-oxide/manganese oxide alloys for UV detectors.

Physicist Eleftherios Iliopoulos, of Boston University,

discussed Molecular Beam Epitaxy (MBE) growth of

III-V nitride films, particularly alloys of gallium-nitride with aluminum-nitride and indium-nitride.

Finally, materials scientist Karl Ludwig, of Boston University, made a brief presentation on behalf of materials scientist Charles Eddy, from the Naval Research

Laboratory (NRL) in Washington, DC, who was unable to attend the workshop. Eddy reviewed plasma

processing and showed that, while much has been

learned about the chemistry of the plasma and the

gas above the processed surface, relatively little is

known about the actual structure of the surface itself. In this case, as in many examples presented

throughout the workshop, the new real-time facilities being planned at the NSLS would provide many

opportunities for enhancing our understanding of fundamental materials processes.

 -Karl Ludwig, Randy Headrick, and Chi-Chang Kao

Workshop Participants
2002 Activity Report 3 - 22

The workshop on advanced detector development was

well attended, with 45 people present. Eight speakers made presentations on pixellated detectors, spectroscopy detectors and other advanced detector developments.

BNL physicist Pavel Rehak presented his ideas and

initial results from a 2-D detector built using Complementary Metal-Oxide Semiconductor (CMOS) readout circuits formed directly on a detector-grade silicon. Rehakís ideas could be used to construct efficient direct-detection devices with rapid (about one

millisecond) readout.

Physicist Paul Seller, of Rutherford Appleton Laboratory, in Chilton, U.K., gave a summary of European

efforts in the design and construction of pixellated

detectors. He described several projects in various

stages of completeness, and left a definite impression that the European synchrotron community may

have been quicker to realize the need for advanced

detectors than their American colleagues.

Biophysicist Mark Tate, of Cornell University in Ithaca,

New York, described the construction and applications of a high-speed (microsecond) pixellated-integrating detector for real-time imaging, and showed

some fascinating data from radiography of vehicle

fuel injectors in action.

BNLís Instrumentation Division scientist Gianluigi De

Geronimo described the design and initial tests of a

384-element spectroscopy detector for use in Extended X-ray Absorption Fine Structure (EXAFS) experiments of dilute systems.

This theme was continued by engineer Chris Cox,

from Princeton Gamma-Tech - a leading supplier of

microanalysis systems for x-ray and gamma ray spectroscopy - of experiments to study incomplete charge

collection effects in lithium-silicon detectors when

used in the soft x-ray range.

Physicist Stephan Friedrich, of the University of California, Davis, described a new class of detectors based

on cryogenics. He showed data from experiments

using superconducting tunneling junction detectors

in the soft x-ray region, demonstrating extraordinarily

good energy resolution, in the range 5-10 eV at a

few hundred eV.

Physicist Dan Fischer, from the National Institute of

Standards and Technology (NIST) in Gaithersburg,

Maryland, described his application of efficient multilayer-based dispersive optics to the problem of extracting a weak fluorescent signal from a large background of other radiation, without requiring an ultra-high resolution detector.

The final talk of the workshop was given by BNL physicist Graham Smith, who described a range of new

ways to perform electron amplification using

micropatterned electrodes. This new technology

should allow optimizing new devices for synchrotron

facilities.

 -Peter Siddons

Advanced Detectors Development Workshop

May 22, 2002

Workshop Participants
3 - 23 Year in Review

ìOn behalf of the Department of Energy, I am pleased

today to officially announce our approval to begin

the conceptual design of the $85 million Center for

Functional Nanomaterials here at Brookhaven.î With

this statement, U.S. Secretary of Energy Spencer

Abraham declared last Friday, June 14, that DOE will

establish a Northeast center for nanoscience research

at BNL, as one of five such facilities to be built around

the country under the National Nanotechnology Initiative.

The study of materials the scale of billionths of a

meter (or 1,000 times smaller than a human hair),

nanoscience is expected to allow researchers to design materials tailored to specific needs, such as

strong, lightweight materials, new lubricants, and

more efficient solar energy cells.

Abraham announced this good news ó BNLís first

June 14, 2001

Secretary Abraham Gives Go-Ahead for BNL Nanoscience

Center

scientific facility construction project since the Relativistic Heavy Ion Collider (RHIC) ó at a Lab-wide

meeting in Berkner Hall, during the Energy Secretaryís

first visit to BNL. Abraham delivered his remarks after touring the Lab with BNL Interim Director Peter

Paul, U.S. Representative Felix Grucci (R-NY, First

District), and DOE Office of Science Director Raymond

Orbach.

The design and construction activities of the

nanoscience center at BNL are expected to start in

fiscal year (FY) 2004, with commissioning planned

for FY2007. The projectís preliminary cost estimate

is $70-85 million. Under DOEís Office of Science, the

conceptual design report will be prepared immediately so that construction funding can be requested

from Congress.

A standing ovation followed Abrahamís announce-
3 - 23 Year in Review

ìOn behalf of the Department of Energy, I am pleased

today to officially announce our approval to begin

the conceptual design of the $85 million Center for

Functional Nanomaterials here at Brookhaven.î With

this statement, U.S. Secretary of Energy Spencer

Abraham declared last Friday, June 14, that DOE will

establish a Northeast center for nanoscience research

at BNL, as one of five such facilities to be built around

the country under the National Nanotechnology Initiative.

The study of materials the scale of billionths of a

meter (or 1,000 times smaller than a human hair),

nanoscience is expected to allow researchers to design materials tailored to specific needs, such as

strong, lightweight materials, new lubricants, and

more efficient solar energy cells.

Abraham announced this good news ó BNLís first

June 14, 2001

Secretary Abraham Gives Go-Ahead for BNL Nanoscience

Center

scientific facility construction project since the Relativistic Heavy Ion Collider (RHIC) ó at a Lab-wide

meeting in Berkner Hall, during the Energy Secretaryís

first visit to BNL. Abraham delivered his remarks after touring the Lab with BNL Interim Director Peter

Paul, U.S. Representative Felix Grucci (R-NY, First

District), and DOE Office of Science Director Raymond

Orbach.

The design and construction activities of the

nanoscience center at BNL are expected to start in

fiscal year (FY) 2004, with commissioning planned

for FY2007. The projectís preliminary cost estimate

is $70-85 million. Under DOEís Office of Science, the

conceptual design report will be prepared immediately so that construction funding can be requested

from Congress.

A standing ovation followed Abrahamís announce-
2002 Activity Report 3 - 24

Spencer Abraham (below, left), Peter Paul, and BNL Associate Director for Basic

Energy Sciences Richard Osgood.

At a press conference held after

Secretary of Energy Spencer Abraham

announced DOEís support for the

nanocenter at BNL: (from left) Director

of DOEís Office of Science Raymond

Orbach, U.S. Representative Felix Grucci,

Secretary Abraham, and BNL Interim

Director Peter Paul.

ment as the audience of BNL employees, facility users, and other guests showed its enthusiasm for this

new scientific facility, which will allow BNL to become

a major player in the new field of nanoscience.

ìNanoscience offers the potential for a second industrial revolution,î Abraham said. ìThe implications

are enormous. That is why we are so serious about

Americaís leading the way in nanoscience.î Grucci, a

member of the House Committee on Science and a

leader on science issues, introduced Abraham, citing

the Energy Secretaryís strong commitment to science policy from the time when he was U.S. Senator

from Michigan, 1995-2001.

ìAbraham was widely viewed by his colleagues and

most observers as the senator with the most and the

best understanding of high-tech policies and issues,î

Grucci said. As Abraham elaborated, the new center

at BNL will be a user facility open to researchers from

across the country and around the world that will

gain access to its state-of-the-art instruments and

equipment through a peer-review process. ìWhen this

center is complete, physicists, chemists, material scientists, and biologists will work with computer scientists and engineers exploring the world atom by

atom,î Abraham said. ìYou need major facilities for

this kind of work, major facilities with the best new
3 - 25 Year in Review

Secretary Abraham (left) learns about the U7A beam at the National Synchrotron Light

Source (NSLS) from researcher Daniel Fischer, NIST; and NSLS Chair, Steven Dierker

(right).

technology and the best minds America has to offer,î

he continued. ìWe have all of this here at

Brookhaven.î

In his welcoming remarks, Paul had emphasized the

Labís role in pursuing forefront scientific research,

both fundamental and applied, and reinforcing collaborative efforts with other scientists, from both research institutions and industry. ìOur motto is ëa

passion for discovery,í î Paul told the audience. ìWe

work with a passion for the science and the sciencebased applications that derive from it for the good of

the nation and industry.î Abraham acknowledged that

nanoscience is still a basic science with no clear applications yet.

But he expressed his commitment to supporting basic science because of its unknown ultimate applications. ìWhat is so exciting about the work we do [at

DOE] is that we produce benefits to America and the

world that go well beyond the original scope of our

mission,î he said. ìNo one really knows where

nanoscience will ultimately lead us, but we do know

that we are at the beginning of a science initiative

that may change the way we look at, and can use,

the world around us.î

Before the all-hands meeting, Abraham, Grucci, and

Orbach, with the Secretaryís wife, Jane Abraham,

Frank Crescenzo, Acting Manager of DOEís

Brookhaven Area Office, and others had toured some

of the Labís main facilities. After receiving an overview of the Lab from Paul, they listened to a lunchtime presentation by Nora Volkow, Associate Laboratory Director for Life Sciences, on the Labís positron

emission tomography facility and the proposed cyclotron isotope research center. Following lunch, the

group toured the RHIC tunnel and STAR detector,

accompanied by Thomas Kirk, Associate Laboratory

Director for High Energy & Nuclear Physics, and others, and learned about BNLís national security and

energy research from Ralph James, Associate Laboratory Director of Energy, Environment & National

Security. The visitors were then shown the NSLS by

Richard Osgood, Associate Laboratory Director for

Basic Energy Sciences, and Steven Dierker, NSLS

Chair, including an overview from Osgood of the thenproposed nanoscience center. ìWith RHIC and with

the nanoscience center, which we launch today,

Brookhaven is on track to remain one of Americaís ó

and the worldís ó most valuable centers for scientific research,î Abraham concluded.

 -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - June 21, 2002.]
2002 Activity Report 3 - 26

Yongjae Lee, a postdoctoral fellow in the Physics

Department, has won the 2002 Alvin Van Valkenburg

Award for his work on a newly discovered class of

materials that expand under pressure.

This award is given every second year in the name of

physicist Alvin Van Valkenburg, co-inventor of the

diamond anvil cell, to honor a young scientist who

uses this device in his or her scientific research.

Lee was presented with a prize from the Alvin Van

Valkenburg Memorial Fund and gave a short talk on

his work at a June 26 awards ceremony hosted by

William Bassett, Cornell University, during the biannual Gordon Conference on ìResearch at High Pressureî in Meriden, New Hampshire, June 23-28. The

award news will also be featured in the upcoming

issue of Physics Today.

ìI am very honored to win this international young

scientist award in high-pressure sciences,î said Lee.

ìMost of the discoveries and results would not have

been possible without support and creative input from

my many mentors and collaborators and the optimal

instrumentation available at Brookhaven Lab.î

Funded by DOEís Division of Materials Sciences and

Division of Chemical Sciences, as well as by BNLís

Laboratory Directed Research & Development, Leeís

research is on the pressure-induced swelling of

zeolites. The phenomenon was discovered

by an international collaboration between BNL and the School of

Yongjae Lee Wins Award for High-Pressure Research

June 26, 2002

Chemical Sciences at Englandís University of Birmingham.

When subjected to great pressures in a diamond anvil

cell, these zeolites expand as fluid from the surrounding medium is squeezed into their tiny pores.

This unusual result may lead to applications for these

materials as ìmolecular spongesî for soaking up

chemical pollutants or even radioactive waste because, when the pressure is released and the material contracts, the fluid and possibly larger molecules

or atoms could be trapped inside.

Using a technique called powder diffraction at the

NSLS, Lee and his collaborators were the first to decipher one such zeoliteís molecular structure last year.

Their findings, published in the Journal of the American Chemical Society, for the first time explained the

materialís unusual ability to absorb excess fluid, and

showed where the extra liquid goes.

Lee came to BNL in 2001 as a postdoctoral fellow in

the powder diffraction group led by Thomas Vogt of

the Physics Department, after completing his doctoral studies in geosciences at Stony Brook University. Lee had received a masterís degree in geosciences from Stony Brook in 1998 and a bachelorís

degree in earth system sciences from Yonsei

University in Seoul, Korea (1996).

Among other honors, Lee has been

awarded a Certificate of Excellence from

the BNL Interim Director during the 2002

NSLS Annual Usersí Meeting, a Sigma Xi

Award for Excellence in

Research at Stony Brook

in 2001, and the Pauling

Prize at the 2000 American Crystallographic Association Meeting.

 -Karen McNulty

[Editorís note: Reprinted

with permission from the

BNL Bulletin - August 23,

2002.]

Yongjae Lee is seen with the diamond anvil cell that he used during the experiments on

zeolites that expand at high pressure.
3 - 27 Year in Review

both adults and children  was shown at 10:30 a.m.,

noon, 1:30 p.m., and 3 p.m. every Sunday during

the summer program. Tour hours are between 10

a.m. and 3 p.m. Admission is free and no reservations are needed, but, to be admitted on site, all

visitors age 16 and over must bring a photo ID.

[Editorís note: Reprinted with permission from the BNL Bulletin - August 9, 2002.]

Despite evidence on walls and mirrors to the contrary, childrenís fingerprints can disappear faster than

those of adults. This little-known fact can hamper

investigations of kidnapping cases, which have been

so prevalent in the news this summer.

But, this summer, this mystery has been studied at

BNL: Lara Hershcovitch, who will be a senior at Mount

Sinai High School this September, is using an infrared microscope at the National Synchrotron Light

Source (NSLS) in an experiment to determine why

adultsí fingerprints can last longer on objects than

childrenís prints do.

BNL Community Summer Science Program: Mount Sinai HS

August 16, 2002

Student Studies at the NSLS

Hershcovitch is a participant in BNLís Community

Summer Science Program, managed by the Labís Office of Educational Programs (OEP) and funded by

Brookhaven Science Associates.

Through this program, 26 high school students have

been spending six weeks at BNL this summer in

hands-on workshops or, as is Hershcovitch, in a research internship. All students also attend morning

lectures on various scientific fields.

In her experiment, Hershcovitch is using the infrared microscope to study fingerprints from fathers and
3 - 27 Year in Review

Despite evidence on walls and mirrors to the contrary, childrenís fingerprints can disappear faster than

those of adults. This little-known fact can hamper

investigations of kidnapping cases, which have been

so prevalent in the news this summer.

But, this summer, this mystery has been studied at

BNL: Lara Hershcovitch, who will be a senior at Mount

Sinai High School this September, is using an infrared microscope at the National Synchrotron Light

Source (NSLS) in an experiment to determine why

adultsí fingerprints can last longer on objects than

childrenís prints do.

BNL Community Summer Science Program: Mount Sinai HS

August 16, 2002

Student Studies at the NSLS

Hershcovitch is a participant in BNLís Community

Summer Science Program, managed by the Labís Office of Educational Programs (OEP) and funded by

Brookhaven Science Associates.

Through this program, 26 high school students have

been spending six weeks at BNL this summer in

hands-on workshops or, as is Hershcovitch, in a research internship. All students also attend morning

lectures on various scientific fields.

In her experiment, Hershcovitch is using the infrared microscope to study fingerprints from fathers and
2002 Activity Report 3 - 28

once again before they start working (in earnest) on

the 2004 budget. Simon Bare and Leemor JoshuaTor represented the NSLS during the visit on September 16-17. We came to realize that this would be

a tough budget year, but we stressed the crucial need

for an investment in the physical sciences, and the

importance of an efficient and productive operation

of the light sources facilities for future growth of the

economy. The point was made that nearly 50% of

growth of the U.S. economy in the last 50 years was

due to Federal investment in scientific and technological innovation and that, now more than ever, we

must not let that falter. We also explained that, because of essentially flat funding for operational support for the synchrotrons for more than a decade,

the DOE is not getting its full return on its investment since the synchrotrons are not utilized to their

full potential. We took this opportunity to meet with

We also visited the offices of Senators Hillary Clinton

and Charles Schumer and the office of Congressman

Felix Grucci. We presented each of them with a framed

photograph of the NSLS with a personalized dedication from the NSLS users thanking them for their

support.

Our trip ended with a meeting with Ray Orbach, the

Director of the Office of Science, and Pat Dehmer,

the Associate Director of Science for Basic Energy

Sciences at the DOE. We updated them on our visits

and discussed other issues important to users such

as the PRT/CAT issue and plans for upgrades. We

also wanted to ensure that our lobbying efforts would

indeed benefit our users.

-Simon Bare
2002 Activity Report 3 - 28

The UEC is vigorously continuing its lobbying efforts

to increase the budget of the Office of Science at the

Department of Energy, which funds the operation of

the four DOE-run synchrotrons, and thus increase

funding for the light sources. The feedback we are

getting is overwhelmingly positive, owing largely to

these grassroots efforts. During our spring visit, Richard Mertens, the Chief of the Energy Branch at the

Office of Management and Budget (OMB) invited us,

representatives from the four synchrotrons, to return in September to update him and make our case

once again before they start working (in earnest) on

the 2004 budget. Simon Bare and Leemor JoshuaTor represented the NSLS during the visit on September 16-17. We came to realize that this would be

a tough budget year, but we stressed the crucial need

for an investment in the physical sciences, and the

importance of an efficient and productive operation

of the light sources facilities for future growth of the

economy. The point was made that nearly 50% of

growth of the U.S. economy in the last 50 years was

due to Federal investment in scientific and technological innovation and that, now more than ever, we

must not let that falter. We also explained that, because of essentially flat funding for operational support for the synchrotrons for more than a decade,

the DOE is not getting its full return on its investment since the synchrotrons are not utilized to their

full potential. We took this opportunity to meet with

other officials, such as Kathie Olsen, the new Associate Director for Science, and Michael Holland, a senior policy analyst, at the Office of Science and Technology Policy (OSTP). We also met with professional

staff members of the energy subcommittee of the

House Committee on Science. We expressed our enthusiasm for the ìBiggert Billî (HR 5270) in the House,

which calls for a substantial increase in funding for

the Office of Science of the DOE. Though there appears to be sympathy for our mission, we as a user

community cannot be complacent at this time.

We also visited the offices of Senators Hillary Clinton

and Charles Schumer and the office of Congressman

Felix Grucci. We presented each of them with a framed

photograph of the NSLS with a personalized dedication from the NSLS users thanking them for their

support.

Our trip ended with a meeting with Ray Orbach, the

Director of the Office of Science, and Pat Dehmer,

the Associate Director of Science for Basic Energy

Sciences at the DOE. We updated them on our visits

and discussed other issues important to users such

as the PRT/CAT issue and plans for upgrades. We

also wanted to ensure that our lobbying efforts would

indeed benefit our users.

-Simon Bare

UEC Lobbying

September 16 - 17, 2003
3 - 29 Year in Review

On Friday, September 21, the NSLS had its annual

Awards Ceremony and Picnic. This year, the festivities were highlighted by a pig roast instead of the

traditional barbeque, an excellent suggestion by

Boyzie Singh. The picnic was coordinated by Laura

Miller and executed by a number of NSLS staff members, including Charlie Nielson, Boyzie Singh, Bob

Best, Joe Greco, Paul Humbert, Jim Lacy, Phil Marino,

Jim Newburgh, and Tom Seda.

This year, Service Awards were given to 20 NSLS

staff members: Charlie Nielson (35 years); John

Smith (30 years); Wayne Rambo, Malry Tardd, Peter

NSLS Annual Awards Ceremony and Picnic

September 21, 2002

DeToll, Bob Kiss, Bob Malone (25 years); George

Jahnes, Norm Cernyar, Randy Church, Li Hua Yu, Tony

Kuczewski, Al Borrelli (20 years); Michael Santana,

Ron Beauman, Joe Greco, Andrew Mingino, Yoong

Koh, Roger Hubbard, Jr., Tom Seda (10 years).

Spotlight Awards were presented to NSLS staff members for the completion of extraordinary accomplishments that were of significant benefit to the Department, Division, or Laboratory. This yearís Spotlight

Award winners were: (1) Bob Best, Patrick Moylan,

Leonard Santangelo and Michael Schwarz for the reduction in Mini-Myte solenoid valve replacements

which decreased machine and beamline downtime,

(2) Michael Caruso for the timely design, assembly,

and testing of a new joint system for a failed critical

vacuum joint, (3) Ken Koebel for leading the NSLS

Budget Group during the time period between Budget Group heads, (4) Michael Lehecka for designing

and constructing a low-profile multi-axis alignment

platform for magnet positioning, and (5) Corinne

Messana for coordinating an important NSLS conference.

NSLS Chairman, Steve Dierker, presented the Service and

Spotlight Awards at the Annual Picnic.

Photo on left: (from left to right) Jim Lacy and Nick Gm ̧r

(NSLS), and Ken Sutter (MSD). Top photo: Staff enjoying

the pig roast.
2002 Activity Report 3 - 30

The first ever NSLS hands-on EXAFS Data Collection

and Analysis Course was a resounding success!

Twenty-eight students participated in the course held

September 23-25, 2002. The course was co-organized by Simon Bare (UOP LLC), Bruce Ravel (Naval

Research Laboratory) and Syed Khalid (NSLS), with

administrative support by Lisa Tranquada (SFA, Inc.),

and held at the NSLS.

The three-day course was divided into two mornings

of lectures, two afternoons of hands-on data collection using six different NSLS spectroscopy beamlines

(X9B, X11A, X18B, X19A, X23B, and X26A), and one

full day of data analysis. The instructors on the NSLS

beamlines were beamline scientists Nebojsa

Marinkovic, Kaumudi Pandya, Wolfgang Caliebe, Syed

Khalid and Tony Lanzirotti as well as Scott Calvin

from NRL.

The morning lectures were given by Matt Newville

(University of Chicago), Rob Scarrow (Haverford College), Simon Bare (UOP LLC), Bruce Ravel (NRL),

Shelly Kelly (Argonne National Laboratory), Anatoly

Frenkel (Yeshiva University), Grant Bunker (Illinois

Institute of Technology), and Trevor Tyson (New Jersey Institute of Technology) on topics ranging from

sample preparation and data collection to EXAFS data

analysis and interpretation of XANES spectra.

NSLS Course on EXAFS Data Collection and Analysis

September 23 - 25, 2002

The participants attending the course were both diverse in their scientific disciplines and in their geographic location and represented universities, national

laboratories and industry. They attended the lectures

in the morning, then were divided up into small groups

by research discipline to conduct the experimental

part of the course. Each student became familiar with

beamline operation and collected data on standard

materials as well as on samples from their individual

research projects. On the final day, the participants

learned data analysis techniques in a computer laboratory established specially for the course. The participants also enjoyed ample time for informal discussion over coffee and in the evenings over meals

and drinks.

There was a tremendous amount of information disseminated over the three days. All the participants

left the course with new friends and armed with the

basic tools to apply x-ray absorption spectroscopy to

their own research.

The course was sponsored by the NSLS, with partial

support by Oxford-Danfysik and Canberra.

It is hoped that the course will be offered again in

2003 - stay tuned for more information!

 -Simon Bare

Workshop Participants
3 - 31 Year in Review

The 5th International Meeting on the Low Energy Electrodynamics in Solids (LEES) was held in Montauk,

NY (USA) during the week of October 13-18, 2002.

Nearly 100 scientists from the U.S., Canada, Europe

and Asia traveled to the eastern end of Long Island

to participate in the meeting. Historically, the LEES

meetings have provided a forum for infrared (especially the far-infrared) spectroscopy of solids. During the dozen years since the inception of the LEES

meeting series, the use of infrared synchrotron radiation for spectroscopy has flourished. At the same

time, the energy resolution for angle-resolved photoemission spectroscopy and x-ray inelastic scattering has increased to the point that they are now powerful tools for the study of low energy phenomena.

Consequently, it was no surprise that 20% of the

presentations directly involved the use of synchrotron facilities.

K. Alex Muller (Zurich), the Nobelist for the discovery of the high Tc

 superconductors, delivered opening remarks and chaired a session addressing both

spectroscopy in high magnetic fields and electron spin

resonance (ESR). In this session, Laszlo Mihaly

(Stony Brook) described how ESR is enhanced when

coupled with very far-infrared synchrotron radiation

and a high-resolution spectrometer. Jack Crow

Meeting Report: Low Energy Electrodynamics in Solids

October 13 - 18, 2002

(NHMFL) surveyed the capabilities at the National

High Magnetic Field Laboratory in Florida and New

Mexico, including infrared and microwave spectroscopy, and also described plans for new European facilities. Many of the meeting attendees agreed that

the addition of high-field magnets at synchrotron

radiation beamlines would significantly advance the

study of electronic and magnetic properties of materials.

Several sessions addressed electronic band structure,

superconducting energy gaps and quasiparticle lifetimes in correlated electron systems. Walter Hardy

(British Columbia) presented microwave spectroscopy

results on the low energy electronic scattering in the

high-Tc

 superconductor YBa2Cu3O7-δ (YBCO) that

agrees with a d-wave energy gap. High-resolution

photoemission was the subject of presentations by

Jim Allen (Michigan) and Tony Valla (Brookhaven),

who each studied quasiparticle lineshapes in systems

having reduced dimensionality. Juan Campuzano

(Argonne) and Alessandra Lanzarra (Berkeley) discussed photoemission results for high-Tc

 superconductors, including electron-phonon interactions.

Phonons and their interaction with electrons were

also the focus of presentations by the Brookhaven

infrared group (Chris Homes and Jiufeng Tu), and a

Some of the LEES 02 conference attendees enjoying a crisp October day in Montauk.

(LEES í02)
2002 Activity Report 3 - 32

generalized theory for extracting electron self energies from infrared and optical reflectance data was

described by Frank Marsiglio (Alberta).

Charge inhomogeneity was another recurring theme

of the meeting. Sophie DeBrion (Grenoble) described

a study of phase separation in manganites using ESR

as a probe. S. Sridhar (Northeastern) explained his

groupís microwave measurement results for a variety of high-Tc

 cuprates in terms of charge/stripe ordering and inhomogeneity. Setsuko Tajima (ISTECTokyo) used far-infrared spectroscopy to study the

low frequency absorption in La2-xSrxCuO4, and suggested that charge inhomogeneity may explain the

excess absorption observed at low frequencies in the

superconducting state. This excess absorption has

consequences for optical sum rules and calculations

of the condensate energy for superconductors. Dirk

Van der Marel (Groningen) discussed the shift in spectral weight observed in the optical conductivity of

systems undergoing a phase transition. The energy

scale over which the spectral weight shifts is expected

to be a measure of the energetics driving the phase

transition itself. Andy Millis (Columbia) presented a

more detailed theoretical discussion of the f-sum rule

and its application to perovskites. Optical sum rules

are also being used by Dimitri Basov (San Diego) to

understand ferromagnetism in Ga1-xMnxAs and other

magnetic III-V semiconductors. In all cases, accurately tracking spectral weight was dependent on

precise spectroscopic data to very low frequencies.

John Hill (Brookhaven) and George Sawatzky (British Columbia) each described synchrotron x-ray studies of low-dimensional, correlated electron systems.

John Hill used resonant inelastic x-ray scattering to

study electronic excitations, achieving 0.3 eV energy

resolution, sufficient to observe cross-gap excitations

and excitons. In contrast to infrared, the larger

momentum of x-rays allows one to probe k-space

away from the zone center and track the dispersion

of various excitations. George Sawatzky discussed

x-ray absorption spectroscopy, using the facilities at

the X1B beamline of the NSLS, to probe charge order in highly correlated electron systems. The ideas

of stripe order, reduced dimensionality, and high-Tc

superconductivity were nicely tied together in a theory

presentation by Steve Kivelson (UCLA).

Superconductivity in MgB2 continues to attract interest, with increasing evidence for multiple energy

gaps. Leo Degiorgi (ETH-Zurich) used infrared

reflectivity measurements on a mosaic of MgB2 crystals, and detected a rather small energy gap. Ferenc

Simon (Budapest) used ESR and microwave absorption to study electronic scattering and the critical field

for MgB2 powders. Conventional metallic behavior

was observed in the normal state, but the magnetic

field dependence in the superconducting state suggests a significant field-induced normal component,

evidence for critical field anisotropy. Other presentations by Jure Demsar (Los Alamos) and Larry Carr

(NSLS - Brookhaven) described time-resolved studies of non-equilibrium dynamics in MgB2.

Photoexcitation drives the electronic system away

from equilibrium, and the relaxation process is probed

by synchrotron THz spectroscopy. Whether the system was strongly perturbed (Demsar) or weakly perturbed (Carr), the relaxation process pointed to at

least two energy gaps.

Time-resolved spectroscopy was also discussed in the

final session of the meeting. Joe Orenstein (Berkeley) has studied the relaxation of photoexcited excess quasiparticles inYBCO and BiSrCaCuO high-Tc

superconductors using 100 fs laser pulses and THz

pulses. In contrast to s-wave (isotropic) superconductors, the excess quasiparticles do not experience

a phonon bottleneck that typically masks the intrinsic quasiparticle recombination rates. Rick Averitt

(Los Alamos) presented a time-resolved study of

collosal magneto-resistance manganites using laserproduced THz pulses. Optical excitation leads to a

decrease in the far-IR conductivity, corresponding to

a shift in spectral weight into the near-IR. The relaxation mechanism was found to depend on the

magnetic state of the material (via spins below Tc

and phonons above Tc). Time-resolved spectroscopy using pulsed infrared synchrotron radiation was

described by David Tanner (Florida), and results for

both electron-hole recombination (semiconductors)

and excess quasiparticle recombination (superconductors) were presented.

The main conference room at the Montauk Yacht Club was

just sufficient for the nearly 100 participants.
3 - 33 Year in Review

On October 14, over fifteen sons learned about work

done at the NSLS, and even performed their own

scientific experiments. The one-day visit was part of

the national ìTake our Sons to Work Dayî. At the

NSLS, the boys learned that the facility produces light

that can take many forms, from infrared to x-rays,

and this light is used for applications in many fields

of science.

NSLS sons were part of over 50 boys that participated in

BNLís annual ìTake Our Sons to Work Dayî.
3 - 33 Year in Review

On October 14, over fifteen sons learned about work

done at the NSLS, and even performed their own

scientific experiments. The one-day visit was part of

the national ìTake our Sons to Work Dayî. At the

NSLS, the boys learned that the facility produces light

that can take many forms, from infrared to x-rays,

and this light is used for applications in many fields

of science.

Learning from Light on ìTake Our Sons to Workî Day at the

NSLS

October 14, 2002

NSLS sons were part of over 50 boys that participated in

BNLís annual ìTake Our Sons to Work Dayî.
2002 Activity Report 3 - 34

For example, scientists can assemble many layers of ultra-thin films, creating structures with

electrical properties that can dramatically

change depending on the values of an applied

magnetic field, a phenomenon called giant magnetoresistance. Another puzzling property is the

co-existence, in some ultra-thin magnetic films

called half-metallics, of both metallic and insulating properties.

Elio Vescovo, physicist at the National Synchrotron

Light Source (NSLS), has been investigating the properties of these intriguing ultra-thin magnetic films

for the last five years. He uses a technique called

photoemission, for which x-rays generated by the

NSLS are projected toward a sample of thin films,

ceived his Ph.D. in nuclear engineering and a Ph.D.

in physics from the Polytechnic Institute of Milan,

Italy. -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - October 11, 2002.]

Elio Vescovo
2002 Activity Report 3 - 34

Over the past few years, scientists have been developing new materials for information storage applications, often in the form of thin-layered films.

The technology has evolved to the point where individual layers may be only a few nanometers - literally just tens of atoms thick. Such multi-layered structures not only promise to go beyond

the limits of the memory density of current computers, but also display a variety of complex

magnetic properties that scientists are only beginning to understand.

For example, scientists can assemble many layers of ultra-thin films, creating structures with

electrical properties that can dramatically

change depending on the values of an applied

magnetic field, a phenomenon called giant magnetoresistance. Another puzzling property is the

co-existence, in some ultra-thin magnetic films

called half-metallics, of both metallic and insulating properties.

Elio Vescovo, physicist at the National Synchrotron

Light Source (NSLS), has been investigating the properties of these intriguing ultra-thin magnetic films

for the last five years. He uses a technique called

photoemission, for which x-rays generated by the

NSLS are projected toward a sample of thin films,

NSLSís Elio Vescovo Talks On Thin Magnetic Films

377th Brookhaven Lecture

October 16, 2002

and electrons ejected from the sample are further

studied to reveal its properties.

Vescovo is currently responsible for the spin-resolved

photoemission program at NSLS beam line U5UA,

where he has been working since 1995. Vescovo received his Ph.D. in nuclear engineering and a Ph.D.

in physics from the Polytechnic Institute of Milan,

Italy. -Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - October 11, 2002.]

Elio Vescovo
3 - 35 Year in Review

As described in the Scientific Staff Manual, a tenure

appointment constitutes ìrecognition of independent

accomplishment of a high order in the performance

of original research or of other intellectually creative

activity appropriate to the purposes of the Laboratory. Recognition may be earned through significant

contributions to knowledge related to the purposes

of the Laboratory and/or in furtherance of the aims

of the Laboratory, through continuing contributions

of outstanding significance to productive uses of the

facilities, or through outstanding and creative contributions to their design, development, and improvement.î

Brookhaven Science Associates (BSA) has granted

tenure to five more Brookhaven scientists. They are:

Lawrence Carr, National Synchrotron Light Source

Department; Arokiasamy J. Francis, Environmental

Sciences Department (ESD); George Hendrey, ESD;

Alexei Tsvelik, Physics Department; and Rajagopal

Venugopalan, Physics.

Tenure appointments are granted by the BSA Board

of Directors after a rigorous selection procedure overseen by the BSA Science & Technology Steering Committee.

In making tenure decisions, the BSA Board is advised by Brookhaven Council members, who are tenured scientific staff, elected by the scientific staff of

their respective departments and divisions. A description of the accomplishments of each of the five newly

tenured scientists will appear in The Bulletin over

successive weeks, starting this week with Lawrence

Carr.

Lawrence Carr, NSLS

Department

Larry Carr, a physicist in the National

Synchrotron Light Source (NSLS) Department was recommended for tenure for his outstanding research accomplishments in solid-state physics based

on far-infrared spectroscopy.

ìLarry has either brought to the NSLS

or characterized all of the new infrared

experimental sources and techniques

in use at BNL today,î said Steve Dierker,

NSLS Chair. ìHe has assumed the lead

role in all aspects of infrared spectroscopy at the NSLS, from its production

to multiple fore-front mid- and far-infrared scientific programs. The NSLS

infrared beamlines under Larryís control are acknowledged leaders worldwide.î

In addition to his infrared beamline development

work, Carr has made significant contributions to the

advancement of accelerator physics at the NSLS.

In 1998, he made the first observation of coherent

emission of very far infrared radiation in the vacuum

ultraviolet storage ring, one of the two NSLS rings.

While not the first observation worldwide, Dierker

notes, it was the second, and it garnered much interest in the accelerator physics community at large.

Larry Carr earned his Ph.D. in physics from Ohio State

University in Columbus in 1982. He joined BNL in

1996 as an associate physicist, becoming a physicist

in 1998.

 ó Patrice Pages

[Editorís note: Reprinted with permission from the BNL Bulletin - December 13, 2002.]

Five BNL Scientists Are Granted Tenure

December 13, 2002

Larry Carr
2002 Activity Report 3 - 36

On Monday, December 30, Raymond Orbach, the

Director of DOEís Office of Science, journeyed to BNL

to meet with U.S. Representative Timothy Bishop,

the newly elected First District Congressman, who

was visiting the Lab for the first time. The visitors,

who included Office of Science advisor Todd Harding

DOE Office of Science Director Orbach, BNL Director Paul

Welcome U.S. Representative Timothy Bishop to BNL

December 30, 2002

Researcher Lisa Miller, National Synchrotron Light Source

Department, and Raymond Orbach, Director of DOEís Office

of Science.

At the DOE Brookhaven Area Office on December 30 are: (from left) Peter Paul, BNL Interim Director, Timothy Bishop,

then U.S. Representative-elect; Raymond Orbach, Director of DOEís Office of Science; and Michael Holland, Manager of

DOE Brookhaven Area Office.

and Congressional staffer Lee Leshen, were welcomed

by Peter Paul, BNL Interim Director, and Michael Holland, Manager of DOEís Brookhaven Area Office

(BAO).

Highlights of Bishopís brief tour of the Lab included a

stop at the National Synchrotron Light Source (NSLS).

Doon Gibbs, Interim Associate Laboratory Director

for Basic Energy Sciences, and NSLS Chair Steven

Dierker, explained a proposed NSLS upgrade which

will dramatically improve the capabilities available to

the approximately 2,500 researchers from scientific

institutions and industry who use the NSLS for their

research each year. They also discussed plans for

the new BNL Center for Functional Nanomaterials

(CFN), for which Secretary of Energy Spencer

Abraham announced DOE approval when he visited

the Lab last June 14.

Bishop, who was sworn in on Tuesday, January 7,

and Orbach then visited the staff on the NSLS experimental floor and saw research results on osteoarthritis and the makeup of newly formed bone. They

also met with facility-users whose findings about

human papillomavirus may lead to drugs to prevent
3 - 37 Year in Review

U.S. Representative Timothy Bishop at BNLís National

Synchrotron Light Source.

cervical cancer. At their next stop, the Relativistic

Heavy Ion Collider (RHIC), the visitors heard from

Tim Hallman of the Physics Department about the

worldís most energetic heavy-ion reactions which are

recreating conditions that existed in the first few

microseconds of the universe, and they saw collision

events recorded with the huge STAR detector.

Bruce Gibbard, Physics, who directs the RHIC Computing Facility, described the technical effort needed

to accept, translate, and store the RHIC collision

events with thousands of tracks and make them available to about 1,000 users simultaneously. The tour

ended with an overview of BNLís pioneering neuroimaging research on the brain chemistry of addiction, mental illness, and aging, from Nora Volkow,

Associate Laboratory Director for Life Sciences. David

Schlyer, Chemistry Department, also explained some

recent research that includes imaging of awake animals.

 -Liz Seubert

[Editorís note: Reprinted with permission from the BNL

Bulletin - January 23, 2003.]

 	


	


	

	







	














	





	








	





		

	
	
	



	









	










	












 !


"#



$

!%$	"$$#




	$	

&	

'"&#

(	









)
	%
	

	


	

%

"#




	*&	



	!

	


	







+	
	
	
	

 


%


!	"#	



	


 





	





	


	

$



	


	

%	


	$
!



&	#

)
	!


 '
(


	
,


&	##

(	


		!

	''




',-

-'!"'



-
	

	(	

	


!&#
#*


	

./0


	






$


	


	
	



 

	


	



	



	





	



	










	















	




 	
	



	


		

	




	 !"#$
% "&'($
	
$


) * )  + $, -   $
$ $
 

(

)$$)		
$
*(()

	
(+
**',




$.


!
"






$	

#



/

$	!


,$,0((, $	$/)*1

- 
2$/) *34/

-
 5
)"##.$	0",,

-( 	) *34/

*
$ 	+
+
	/)
	((*,+,

$ 5'	) *34/


15$ 
'.')*1*


 	
	)*1


''	 $	
) *34/

 65	 5	)*15	$

7 
$.)*.$	+


			

'$-8
'($$$$
$

	*	
		 ",



	


	$$$%&
$$'

	*/$		,

)	9'/ ,


)*15	$

'	
).$/( ,

8
)9"1 ,

9') ,(2$)

	9)

	

)'9++,

$	$	)931"3

+,) ,


	) ,(()

8++)*

55
)*



.$	.

$%&'

	





 
	



(


 


	


	

6 6 	) *34/

"6$)*1*

7. $)*1*

2(+)*1*

")*15	$

)-

	)*1*

:)99-


 


	$5$8 ++	''

  
 .;
 +   ' + 	 5' 


5,+(	$($$


,

		 	 


	 5' 
 5 %55&    8  5',

+(	$($$


,




$	)*-


$	9(()$

9+/)*

	


	).$/( ,

7
)*

*2)*3 

.
7
)'9+

	


8) *345+
	

.$	.) *34/

	
  

/)3	 ,


9
) ,(8



)*-,(
$	,

	


9) *34/

.+)"##+


) ,

		!	"#


	 8  :	   '
 + 8

 )5.
)*((,



 :5

/	$

+"($



*	 ,

+-

 ,(2$

 	




	

				

	
	

	
	
			

	



	

	
	



		


			

		 



	! ""!  #

"" "	 
 "	"

			$%		

		&

● !'"	!

"	 

""	"

	"		"

● 
		 "	()	*!+

*
!	))
"*

● ""			

 	 "	*





%
					"		

"   *  	 	 

"	*  	 	 
*$  %  

 "	( 	 , %	 	 "		 "

"*	-./0!""	
*

(12
*$3		

"		"*$% 

	(*
1#2	""	
!

"	
"'	""	"	

((	$%	
*

 	  	 4 " 	 "

"5"		


*  5 
	 	 	 "$

%*						

	
*"	(!
""

"
*	!)6"7

'		"	

($%	5"*1892		

 :  	
 6	"7!  89 

* 	  " +  	
 89 "$

% *" " 	 	 ""	 "	

(! " "! ! 	"! 

"		!	'*		!
	

,
			"	"		$

;'	'	"	*

 	 	  	 

"	!" ,

5	<+

"	"
$		

!'"	

	 	  
 # =

>	! 1#=>72  "	'	

	
/""	>

""		 !	

	'*
	

	$

%		? 

'+	'		*!

	
''	
$"**	


(	"@


	   
 	" 	

						!
	

" ( 	 	 	 	 	

	$


	 '* 1		  "

2'*1		 "	 	 	

"2	*!

 	
 8;	">

!4!
		 	
 

'	
$
.>.!


		'	


A)			
/!

'"	89

'!
"4)					$/

	
*	
!


B	*"		*		

		,	$

	
	
			
		

	
 



 
	
 			

	

 	

 	
		



 		
 

	

	
 	
	
	

 	



	 


	
 !

"#




  

	 
  


 
   


   




 

 !  	 	  ' 	

	B"!
6	7	

5   	 '	$   
 

""		
	"

' 	<:! 	 			 <+

"  " 	 (   	

$ 	(


*  	 	  '*!   


89"*<:"		$

%	"		<:	


	
*	
#=>!	'

"	 "  	 	  	 	

"	"		 "$


				>.

9  	 	  	 	  3>

*!(			"*

	"9 !"	"	

		-=-=*		

	"$

/			!"	

	"		B"'		"	


	! 		 "	

*$3	B"
*		


		"		"&

● #:,C'*			

● 
""			1

"2

● >5	"			

1,	*		2

● >5	""

● ;	!""		

			B"

	'B"!		
	B"


 " 	 DA $   	

 	B"   	 	   	!

*  	   	  "$

%	  
 '	 "* ' 	 	 

"	*"$

 		!	
	!

	
	 "	*!

	   	  ( 	 	  

"*$	**"!'


		*	

	"	"("!

	'				"	*$

		

	




	

	

	


			









	






			

	
	

		
	 


		



 


	

!"#$%%&


'(


!"#
$%&'
&

")		*	




%+)	

+&*
)*	

,	%



%&"



!"#$	&


!('
)	


	-"	

					

!(	
+

*)*+

,)	


!(%		

-#)./
'
&

	
	

.	

/)	)+!

+&	

+&.	

"$

-

)	


+&&

*%)

 	




	


	


	
	
	

	



	

  		

  









  
   

 !"#$%&$'



	
(


 		

 	 	
)

 *+,)  

'

- . /
		
)

 #0$


	

		

&	
)


 ) 
 
		 


&
	$

		

 '&


"(

● 
1

 

	
"


2

		


(


2' 	"



3

● &

%
%"



 3

● &
	&

&3

● &""

	
&

"
		


	

&

	)$$)
&




	



45'672&"
$





  
 "
  "& 
 
	


"1

 
		

	"&
2


	
&"
8
 "	
'

&"$%
	)
'


& 
 



 	8  
" 




	$
  
"


	"&
$/

 )'




	
 2&

	"	




	
"&"



	8 '


"	

 
 "8








	
 $
)8	


	


 
 
 9&
  7


)
&"&
"
'




	8 
"

$: 





	8 
"	
(

 	


  
  
 "  " &


"
		
3"&
	
	'

	


"3	&


"	'


	3"
	


	"&	
 
"$

		

9&


. 7  
 '



	"	


 
 	
 

  
" 


 
 	
	
  

	""	

 



"'

	 "
 5%7 $

  
" 	
 

 
 "

&
"
"
 


		
)    
 

"&
;&

8

)



		

2	



"

  


		
$

545




	8


&

 $<'
'




	

)	
"

&




	

)	

 

)

"

 
 
2

     
 



$=

2'  
"	

 	
&'

"




	
		

"


"
$/&
	
)
'
&'

	




 
"		
'



	

"
)	&

&'


  &
" ) &" 	

 







 
"$ 
"


 & 
    	
  &&
 


	

	$=,8
"8


2' 

 
"&

	


 >$

/)
%
	%"

	'


  "
)"  "" 


"
	 
2
"'&

)	



%?4'@$  "
       
 

"

&&

	
	"'


)	
	"&

$%?4'@






% >


''

1	 		

	

*@

	'



2' )
&
	 

'


&"
 


/




A

$




 

0 2 4 6 8 10

100

104

1

10

105

103

Distance [m]

Signal [pJ]

FEL Light

SASE Signal at DUV-FEL February 2002

l = 400 nm

BW ~ 2 nm 

Gain wrt Spontaneous ~ 104

0 2 4 6 8 10

100

104

1

10

105

103

Distance [m]

Signal [pJ]

FEL Light

SASE Signal at DUV-FEL February 2002

l = 400 nm

BW ~ 2 nm 

Gain wrt Spontaneous ~ 104

Gain length LG=0.9 m

9
&+	
	
(

● 
 
)
&






1'&	"
 )


&
	
*
2' 



● 
 &		
)
'&







2' 


'85
&
2' )




&&4&

● 0
	&



		



B
%
08)B
)
	


	#8
 )B
)


	0
	)/

)

	


&&


&
"
7'

 97	
&"


&		
 



● %
	&&&"
'"


)'	")2' 


&
	


*C


&" "&

2&


&



	
$2'



"


1
  	
  $ 

 
  	
 


&

2	&




 
2)
 

	
& 
'


	$

"



	



1


&"


	

3



) 	 
	)


	



	&





$	






	""
  
  
 1"
    

	 8
97 
  

 




97D
'
"&
 


	

$

	

))
		8


45'672&"

&	


	

	
	
	&&
	



	""
 $45'67
'


 	
1	 &
+	


 
'



"&&
 
"	

&
	
"





		

)

	
D 	


 %5$  
 
  &8 	
 '

1
67)'"
				"'

&




"&


	'

	

$

67
)

	


" 
  '"
 
 /4 



/	

4

 
"$

/)
"&"



45'67$/6 )
67
&
'

 
'"&
 " 7 
 E "'


 
    $ 7 
 << "





<C	
"
1

 

"
)

)&
") 



	"


67


<<'"


 " 
 

" &&
'

$

/

1
)

8



45'67


  	

 
&



"
	&
	A?A"	?'


 A?A? 67$
 	"&

  
 A?A?





9	
)A?A?
'



<<"

F''

"

)""
&'

"

		

A?A?
&
'


	"8
&"	

 $

 "&

 
  	 

  


A?A?67





"	F@

"





 


  &	
  
 

  
 << "'


$

4
67

&"

	"
 

2&"
 	"     
 F@''

"



&"&"&	
'

	& $  
# 	"
  "

 &'

&

2&

&



45'67'


$

 545

& 
45

67 	"&
"
  
 
545  	 

&
	""
 $

MGU RF CAVITY 

#4

RF CAVITY 

#3

	





  	  	    

 !
"
 	

	

	



	


	
	
			

	



	

	
	











 








	


 ! 	

" 	



  


#

● $ 	


	 


	

	 


"

● %

	


	

& 

● '	




	& 

● (





"%	

	
	&	

"





	


	
#) 




*+"),
-./ 
0	

*
 +
-. $ 
 
&   &&

*
 1-. 	


	 2  && *(

2
3-.	,*2
-






.
& ".

	
	




 	




	3&& %	
 



 &
	3&


	 	 
 
   
" 

 
	
	.
& "

	%&
 	
43&


  
  
 &
  

" 

	


	&&

	 

.


 	5
&     	


	




& .

 
&&
	



&



&!	"
	


	 '
 *'-.  &   6"

*06-.& *0-


		

" 
	 
&	
.



&	 .


%"&	 . !	
	

	& 	 

/

. 
"'

	 	.  ,
 

+
2&
(	


6	
	*,0+2(6-

,  6

  +	

 	
	 *,6+-.  


"$3


"

"
%&
 

	&




		



&	

	
   		   

	7%&	

	 	. 
 
  


"		
/


1*/1-		.


  	&
 	
	



 	
		 



&

    %&
  	
4  


		
	



/ 

 
	
     
  "  

	 

.


 !&

 89&		

 


  		
    %" 
	&




) &   &   
 	 


	2"&" 



.	 

" 


6%&
 2"
	/


, "  *62/,-    


"	 	


.


	
"





 .  
 8$. 8)  : 

&    62/, 	 " .

	 && 


8;8$ 
8$.8,.8<,.8:.8=)

8=,&
 

	 * 
" /1- 
 ;.  
8

8;
&
	 &&	


  , & 
  &	   89

& 0  
 
  &  

	



		
&

 "	&&
	

	"

  " 	 	
 

	7 
  
		

	 

 

	
0 


	

	
&
 
68)'8)6&	

	&"
 "  .




">
&	 

	
 	
 	
.
	
"  

  
  	
  	&

" 

	 "    "  
 
  

	 
	
	
.
		&
;

	  "  
 	 &" 	 &	

.     
 
  



 
&




	

&

) &"& 

 ?= 	 
 &
 


		

 




&
	
 



   

	7 
   &


	

			



7

&	


		
>: 


	
&.
	&	4




 ;+1*-

	
&


  

   
  
	 



	 	   	  	 



	
&
.& 


(@
A 

%

"	 /&
	., 
 A
	






4
"



	


	
 
7&


	"

 	 		"&"	 
"

   % " &	

.   


  
" 		   $
"	 &

 
 0	    &  &



 &	
	

	
""	  !

&1
.
 .


&

 



	 
 

3

"%&


 .3

&

 

	  &&


"".&&		

8? 
." )6

,

+
	
.$$
"& ..

!
""/106.


	. 	 		"

&" 

%&	
&

>

)"	

 "

	

&
	


		 

 
".  %&	       


	
" 
   %&
 "	 



	
4.


&

& 	

"

		

"	


	
	.


	
&
	
		 

 
"/&	
.






& 		&
	"

     
  & 		 

 
 &

&&

&
	".	


&
		



	 
"06"

	 	


.
%&	
&	"

 ;/&
	

	&
	".  
&



&


& ) 

 .

 &     
   

	
	




"

'
".
3
 
 


&		
	'
.

	68)'		
"



& "%&
	 

3& 
 
	3
"		

	B(&
,	
	



.C	

"

$ $
" &   	 	 	"

&"'	368)'	

% "&




	 


. 	



	.	"	&&& 



& &






 .5	"  .&

 


%&
 . &

%	

.	
	

	

3"		&
	
"

'.




	&	

 



&		
&&

	
4.&&"
 
 .		



%&
 

	



	




	


	
	
	








		


	 




!		
 	




	
		




	


	
		



		


	




     



 
   


		



 
		
!"#$	


 

 


$%&'(#)
*





+
 
  

 


		



	
 $"& 
	 
 
	


  
	

 	 	
	 



 $)& 	 
	, 



 -& 

	 

 -& 

 	


.&	

	
	/&


	,
	
,
	
0
	


  
 	 	

	
   

 	



	
	
	
	

		


	

	


	


 
 
 	 	
 1
	 

	

	


	


	

	 
, 






	

0

	

	





	2	


    	
   
 #))) 

 	 

 	
	 		 	  	
	

		
3
	
	



	    	
   ##%$ 




+4%!3	

	""&

	   	 5  
 



	
	

3
	

 	  	 5  
	,
	
,


	
'#)&*
		

'#.&*



	

')&*

,
'-&*

	

	
'$&*	



	

'!&*3
	






2
		5


	2
	

		


		
	


5
	

	

	
	



	 	

 


 


 
	  
	
  
	,






0
		

	




  
  	 

	  	 	  	


 
  	
 


   	
 


6 7
  

6 	





' 7,*5

$"&   	
6 	 

7
 

	  7 


5			/&

	+	
	


	 


  
 



 + '#"&* 8 '#%&*

	
'#!&*

72
 /.&  
 
 	
 	

	9	
	
	
7


		 
    	
 	



'#%&*
 7

	

'$&*



		
'.&*
'(&*	


'#%&*

3!"#$
2
 	
 +4%!	


		  "#/ : 9 	 
 


!..	
	
/)


	$!
	2
	
!/

2
		
	
	$"




+	

	2





	 		 
	
2			



		
	
	



		


'$-&* 
		 

'$$&*

	
	

	
	'!#&*



		  '"&* 	 

 



'"&*


		


1 9
 1
	
  	2 2
	  
;


	

		


 
	 	 	
2	 
 	 	

	
 

	 
	 
 ;


		!%%!
<2


;
	2
	
				
	
;


1
	<		
22


 	
	 	 			 
 
 

=

+
			
	'=+*	
	




 

9
 1
	 	 
   
<

	2

	


    

 	

 
	

 	




 	 	 
	 	 :
< 	 


	


	
		
5

+6
	
:		

	=+	<8

	




	<	
		
	>


 9
1
	
	2




	  9
6 ? 
 
 ?	

	@

=
	
	



	 
 =+ 2    


		2
<


	


	
	
	
	



	


	 	



1     +4%!   	

 



	
 	


#"!#

A9
	 +
 B 	 1C 1 	





	




	
:
3	





		

 
 	  	
	 
 	

   	

	 


  

 	 
<	2

			
	
		'/$#*$""

9>
	
9
1
	7



 3


'/$#*$""()(/
	
2
	

	
2

	2:
	


	
	



	

	



		

	'/$#*$""

9>	6		



 ! "" 

	
	2	2
	





	

  =
	 



	

	

	2		


		
6	


2	
2	



	

2		+


	
	


 	


	


	2


 	




	


	

	
	
	

	



	

 	

 
 


   
 


 


!

"

#	
$	% 
&


#%'(

#	
%	 #	
	&

!#
	##
		
&

	
'()

%!
	


 	
 	! &


 


	
$
	*$#	

	
	#	
!$
	*$


	! 
	*%

%#	&


	$(
	
	



'(
#*## 

	  
 $   $
	* 
  &

#	 	
% ! ! + ,#	

	$
$
	*#%
	%
	
!*


	
  	 % 

	%
 %

	$
!!$%
	%
#!&




	%!#%


!!-	%
 





.##
%
	#
	'(!
&

#	
	!	%/01221 

	
#
	#	
	!!
		

,! % 
	
,#
	$
$


	
-	$
$


3&

	
$%	!

!	




$
	#
!!		
$%!

!	   	 
 ! 
  ,#	&

 

	  	4	 %
  

$&

# '

$	!
$	!

 
  	 
 	 
 
 
	 
	

#
		4			,&

#! 
 

$$$
	*%
  ,#	



	 5!
	

$



!!
$,

#!&




	#	
%	'( .

$
	$
		$!! 

	
65				'(

$  	 
  # 




%! 	   7 
 

	%

	
	
	

&


%!8!5%9
$!
*

#!
	4	
#
&


%%	$

##	
 #	
! ,	 
 '( 

/	
!
#$	4	&

 
 !		  #
 
	

	 %!   	

%
	 !$

	
 $  $ 	 


	
: !

 % 


	


(
	
	:#

	!
	
	7#	
(:
 

/	   	 
    5##	


/
		

!
	##	



	% 	 
 '(
$	 #	!#

	% !
	 

	65$$%!
&


,#	!%	
# !&

$

!	

		4	



#	
-
 

.	!
%	%#	
	
	#



!

%
%!
	
	4	 
!
&

	
	
	
%$#
	
$
	&

#!   5% 
 %! 	
 ,#
	


!!		
	

$!
		!
&

	 
  	4	  
  $ #
	

	%
#	
$%!


'(

	4	 

	65#

!	%
!!
!


	

	!!	!!*

$
!,#
	!	%3

;222

;225!#
$	## 


!

4#
	
	

#	
!	 	
!
#  .&

4#%
!%	

*
$%$
	*%$	!,#


;222< 

 	 
 6 $
 %	 	 		  



	%
!

#
   8)
! =	 5	 6 )



	* >	 )4	 9   	 	%	 




 

% !  $ #
 
	  #	
 ,#	


##
	$
	* 5%
!
&


 , $  ! $		%  #	


	 	 
 !
# $  ,% 	

%!

#
%  	
  	3 #	
 $

!'(>	!5	
5!

	
	


&!
#! $ '(  7 	

%! 	&

4	 

 	  & /
	 %	 	 		  

 
  
	% $  	



	% 5		
%	
#

	#
	
$	%	
%

%

	$
	*	 	
%	
#


$	#	
#	
		!!



,#		
!

			!

#	%'(
	?2 !$


!'(>	!5	
5!

	
	


&!
#!$'(7	

%!

	4	 

.!!
!
!*
!
&

#!$	4	!	&



!
!	
	#	
%	

!	 
  5 , !	4 !
&

!
	#	
$	

  

$%	 
	#	
&

122@+

● A		#
!
#!!	


		%
	,#!


● .!	##
	
	%
%	

	

● .#	


	
	#



	#	


● .!		%
	

● .#	
$
	*#%
		




● .#	
'(!#!!	%

	
$	
	
	%/0

122@  .#	
  
	 #	
	!  



	


		$



	 

 !"#$%

● 	
	
	
						

			 
!			
	

	


	!		
"
#
$

● %	
		 	
			
	

	
		
!
		
	$

● %	
	 	!		
		
		! 

!	
&	'	'			
! 	



	$

● &	
	
	
			
		
			


"
#
				
"
#
$

● 	
! 			
!	
	(

■ )				
	*+,	
		

	
"
#
%	
	-$

■ 	
	 				$

■ )				$

■ )		
!!		
		$

■ )	
!
&	
	$

■ 
	
				$

■ .	!		
	

		
 	!

!		!!$

■ 
	
&		!		!	


	$

■ /00001	
"
#
	'0**+!'

''	$2
'$

■ #	
!		
!
	
		
		


		
!	
		$
 	




	




	


	





 	
 
 
  








 !"#$



%&



'()'$*

+
	
()!",
-

.*
	
#/

 
   

!"
00



 

		


!" 
#1



  !"   








  2
	
2 



	#

	



/
 
   
&


	

00#

3

"	(4$





5
!"

$6
 
#  ! 
  
 &






#,	


 
 
  # %  



	,,+(),
&


,
+
*#4	
"	
&


 

	    


     
   	#

7




	
#

	


+
 #%0$

&



5

 #%8%+%8%4#+&

		%8%+

5"	&



,
4
9
#3


!"


   1
  
 


	"4

&0#!"


!/

,


,   9
#  
 
  

!":+ 


&;

!3
&; 


&0; "
 4

 &+; $


<
 &;  =#<# /
 &

8; +
   	

 &>>;

?

)		*
&>8;

,4@
&%%;'.


&#




     
 


!"


"	
:4

3

&
4
/


3'<


 
 # #  ! A


B

B&

C
'

4$
$



&&>

#

3

13'!"

&#



	 


3!"

-


  
  	
 

#"5






!"
	



#

4-
 
  	  
  = D 8


-
&
&

	C
&A	5

00#

1




#

 
 
  '


9
(C
C 

  

	 #%8%
	6

      
 


 	 

	






5
@#

	


!  	 

		!"
	&





 4&



 

# B

5


&





 
 

	

#,$





 



00







6

#3	&





 #%





  

 '$C  C'. 
  	

'
$
C
)'$C*

C'
.#!&








6

&

#

	

/	
 	
-

=&


00/


 
&   = 
   



-#3



 	     
 
 


 
    4 9 E


)49E*	
	+	
$

C4
 !"( '



!"#$6












= 	 6 
-
   

49E	

=&
 # 3    ,&E $


),E$(*





F+3
&

 
  49E 
 



008#


-

6&


&

00


  

  

 
 
5 )BA* 




G>#3BA












-




  
& B9+ #  1







&




		



=&
	

#+








	



#'(








	 !"C
"BC&



6

&

BA#3






 	  	   

	F+3





=49E#

 ,4
) ,4*


=&


5



  
  

   =&


6
 
# $





	
FEF

&


 
  








#

1
	








!"#/
	






6

&#

	



 

	
 	


 	


	
	


  	

 ! ""#"
##
  	


	
	

 $ ""


 % 
#


! &		
	


"
##
 ' '

""

( (
	



 ' '




$ $"
	
	  &		
	

 #)


#	
 % 
#


*! &		
	




&	  	


	
	

 

 ""

 	


	
		




 ' )


	


 	
 

		
  	   


	
   
 
 
  


 	 

  	 ! 

 "


	#		
	
$


 %"&
 
 '( )*+ ,-- . 
  *

*	 ** 
 (--*+/-.#	"

0




	
"

 	 
 	1"
	"

	 +
  

1"


	
+
+	#





			1

	

	#		#
		

 0'2--


	
3--
"

	
+ 	0 2- 	  			
+ 	 	

!		40
	
		



		



	5


#4+ '3 	  
+ 		  
+ 1


		





.
	

+	
	

	+	0



	
6	
"

	
	
		0


#	#
		
$

)
		6"


&6&)

"



 
0	 
 
 
  

	.
	"

0#		
.		



 0'27	 0

	)
6&		"

 #  
 	 	
 	 	


	
8
6&	
	"

	
	

#	
	





			6&+

+

	
	
	9
+
	+






+		

	#+



2:%"&

',**	"

	

		
#
	1"


  		#
    		





9"



	

	
 	


	

	 	

  	
 
 		 !





  "#$#% &'"$$($)*$

"

+#(


  "#$#% &'$	$ )

"

,  
-  $.

/0/.'$/$%

/'$/$%

$/$%

&  - , $.$%

1.$/$%

$ $$.$%

($.$%

&  
- 

 1.$/$%

- $$$.$%


 2 ./$%


%)( -"$$($)34%


%$$5$


%$$5'$

&"  ")#$#% 
&'1.$/$%

"

 "$ -  $/$%

2. -	 1.$/$%

--	 .$%)4

$#$#%

6  
- 7
 1.$/$%

	
 20 ' '#%

$"$$($)$34%

($.$%

43.$%

.$%)

6  	
 , 1.$/$%

-


-

7  -	 6, .$%) )5.

	


7  	
  "2.

-	 .$%) )5.

.$%)

8  -$$'!#$ *$' 1.$/$%

8   2 
!7!8 1.$/$%

)(

  "#$#% ,'1.$/$%

  " &'1.$/$%

"#$#% .$%)1$0

 #$#$ ,, 1.$/$%

-

#$9$
	



 

	

	 	

  	
 
 



   !"#!#" $%#&

' !"#!#" 
(


)&!!"#!#" !*'

$ ! +& +& 

,#

$ ! -
 .$ !!

,# -/
 

%  	-
 .$ 

-


0  	-
 . 

1!!

!*)2!

	! 
)	3 .. 

,# /223!#4/56


(-!1


(


!*)2!

	 ! 
)	3 . 
(


,#

	 ! 	
 0 !!

,# 	*1!## 

	-
 '78 !1

	!#9# !*:

	  	&#&" 
$. /223!#4/56

	$ 	,9!#! ;9$ *!

"


(1**


(


	$  	,9!#! 0$ *!

3#1#!" "

	
 
(1**


	
 
(


	$ 	,9"< 0$ *!

/	'
 "

	
 
(1**


(


	$  	,9!1*# 00 *!

"


(1**


(


	%  3, $6. 8<81!3# !1

	%5  3, = 8<81!3# !1

	.  !#!# %%=3 

'!#1!71&>1#?@'A

*
!

!


#1!!

!*-!
 	


	

	 	

  	

	
	  
 !!

"#$ 
%&'(	)	


	

	*)'!
+,%	


-  . / '	0		)	
	

  .123  '	0		)	
	

('
	',4')( 2	

5'%	


%06%


 '	 


(	)	1%			
		


*
)		

  7%7. / '	0		)	
	

.1 
)

.1
)
	)

8  ) +/-+9 ')0		

	3 0		)	
	


)	 
0		)	
	

%		0		)	
	

8(  . 9 '	0		)	
	

: 		'


)	 
0		)	
	

0		)
	'(&)(			


(	)	1
)


9  .  )
;
())

))


%)	<!
&(	
	'

9  .  )
;
())

% 0		)!
&
:	)'

;=%

0;=%

  %%  ;>>
)
	',;(+

.1 
)

.123

7%7.

	)

  .123 +/ ;>>
)
	',;(+

.1
&	

7%7.

	)

(  % / ;>>
)
	',;(+

;=%

0;=%

  % +? '	0		)	
	

;=% :&())

0;=% 0		)
	'	
	

.=% 0		)%&	7		(

03@
!
&4')

0'(	)	%	


*	0'3
0		)	
	

*	&)%'!
&

+%+; 	)*


(&
	



 

	

	 	

  	
 

 

 !


"#!$#%

&' ( "#)!*

%
+ 

,"
!( "

+
-,!*!

+ #%!!"

  ./! 01 
234 

  51 
4 

%  51 6

 

 (   !*7  
4844 

1! 5* /! !/

5%1

 (  -!##! 

 

1!

3  17 *!  
2 .*

+ #) 

3  95
) $- 

*/


  1( 83
 *


$ 

"/
!	!

( ( "#)!*

%
+ 

& + 

+ #%


  
 

 "!)!* 7(!

	


	


2  17 "#! 3 "!)!* 7(!

+ #( 7%!*

2  17/& 68
 "!)!* 7(!

17 "#!

2%  
 3

 "!)!* 7(!

17/& + #( 7%!*

6(  17/& 444 

1! %*( "#$ *


+:


6% (  17/& 
84 %*( "#$ *

1! 17 *!  &!-

9*/ " !  !

+ #%!*

8  $
$1 3; 

17 *!  , 
+ 

17 "#! ,""+ 

17/& + #5

#! + #5 "





8  
 
234 
*7(!
 	


	

	 	

  	
 
  

!"#$ 	
 %&'"()"* %+, 

-.%+"%+, 

/""

0'123,"")"* 

%4' 

33/01''50"


&1*'4' 

4' 2%25-'

4' 261" 

4' 2)''

473

8	  	 9:
8  

	
 %&'"()"* %+, 

	
 -.%+"%+, 

/""

0'123,"")"* 

%4' 

&1*'4' 

4' 2%25-'

4' 261" 

4' 2)''

473

8%   '"*5;1 : 	+ &'" 

&-5'12" %*<4' 

 2" -+1%*

 ,*, ='>,'4' 

	1","	*" 

4? 

4' 2%"*

4' 20'5%"*

4' 2@'"'

9	  &-5'12" 
A9 0<&'"-'

 +"22" 4' 2)

9  &-5'12" :
 0<&'"-'

4' 2)

9%  &-5'12"  0<&'"-'

&-5+' 4' 2)

90'  '"'"* 
  

-"  21'""

	

99	  &-5'*" ' 5A9  

&-5'12" &1*'4' 

&-5+' 4' 2< 

 2" 

@	@	-

 '"*5'12"

99   '"*5;1   

&-5'12" >4' 

&1*'4' 

99%  &-5'*" ' A  

&-5'12" &1*'4' 

 '"*5+*" 4' 2< 

 2" 
	



 

	

	 	

 	 

 

	

	

 	

! "#$

  	 
%& !'(

	

	

! "#$

  	) %*
& 

+	 ,'-.	'/0(1


.-'((

	

-1'#('(#

2  +	 3
%* !'(

& ,' 4 
 

 (

3  
5(# 
 


5(..( 6'.2(1

6'.71

32  4 &
 

2	#18

	69	

  
5(51# *

 

  8!4	0 )5 

2  		 % '6	",(:.54;

)	) 8$,

! "5
' ,'-.	'/0(1

,'-'.8

	-.().2

$<','-.0(1

	69	

6	(

*2  
.#1 )5 '21.4(

 	


	







	

 	

	

 	

		 

		
 


  !"	#$



	




	

 	


%	

 &!	

'  (!	

		))* +

,)	-*	.* (/	

	#$	0 (+

		0 (&

%	#$	- ("	

	#$	- (	

%		- !("	

		- (&	

%	 ,)(	

	,)(+	

	 ')("

12	.	 !	

.	
 !( 	#$

#$	 3) (""
4+	4*

	3) "(
4!	4*

	 3) 5(!

	

	

	



 !"!#$%$!

 0
) 6
 -	7289 -:	728;9 -<	728;9 
=	>?	79

-- ,) (// 4&(/& 4! (!

6 6*) + " (  (

6 6*) + /(" (

 %) + (& (
	



 

	

	








	



 



	




	 	 !" #

$



 % 




$&

'	
 


$(


'
)
 *

+",

$(


'
)
 -**%



 .. /!**


& 0 1
 . 






2 3*



2

'	
1
 44 5
6  43


,$

7*89%*+:; 5!


9* +:;&
,




 %.


,
<

#


 <
	
2=

>?2>'



$<	
	
2 0

&

2
 %




+

	


 *0?2	
5




 *<
"	
*





1



 5 0> *!

+

	
 *5%

@==
A

 %*3+:;

@2
29
 *0BC	$&


	


 *

	


 %B B

<

1

  



<	
2 %" > 

D*8

&
,

* .3D*8

*,	9* +:;&
,




 5!


$@=&
 .

1	&
+2
 3

:;
'	
2

 	 !
#2


'	
2

	 
5%
#20
#2

	E

9
	
:;
+2
7 8 5*B

 	y 2F




<
')



  * 
2>G33 
2** 
2

	E

(


'
)




&

=


,   >%0

<
<;
,)  *0 
>G0% 
 


	E

&

=

 (,)  **%> *! 0* 

'	

=

 

, %!*>305.5


 = -’ , #0! 3>5 #.!


  +

,

,35.3> 5 5%

<
<;
 , %5!%! 
 G!G3 
 	
 


	E

<
')



 , !!535 
2> .%!. 

 %%#* 
2

	E

8<




 	


	





	


	




 


	



 



 

 


 
 !"!



#
$
%
&	
 '

#
(


&
) 
 *



(


&
) 
 +,-



./!'*0 !"-."!1
/

./ -0.2/ ,.*!1
/

$ !'*0
.*"-

/


 
#%
3 -*"


 
3

&	
0
 4  4,
 5 4
 

 
6 
.
7


/ 6
	
38
 
9:30	


#
6	
	
3 

!*$

3
."


 /



	


 ,:3	
.,-


 /

!*:3	
.


 /

'6
	
 .


 /


0



 ;9-"



	 
 ,!

<88
=

 > -?@

<3
3%A
$

3


 !;12.-/

<8%
1
 !!1

&

<8%A
 ,-12

6>
 
0

. '



>6	
3 .B/ ;!

$
 

 ./ " 

#
<8$ 1
 '

0>	 $
 3
 -

?@
&	
3
 
 "-!

73


 &	
3
 
 !-!

73

%A
	
?@
3
.-/ '2



(


&
) 
%



$

8
 


 !*9'-

6 
6@


,) ' 9 * 

6 
&)


 
.

	
	/* 39 '- 3

 6 
%



$

8
 
 (, !'9";*-

&	

8
 
	 ,"7!!97';

  	
 7,;!*97',,-




	 ;-;*9!-

6 
6@
 ( '"!*! 9"-' 

6 
&)


 
		 ,"*', 39;"3
 


Unscheduled

Operations

3.20%

Operations

Studies 66.27%

7.56%

Maintenance

15.41%

Com/Con

2.00%

Unscheduled

Downtime

1.95%

Injection

1.13%

Holiday

2.48%

Interlock

0.00%

Studies

8.25%

Operations

55.63%

Unscheduled

Operation

7.57%

Unscheduled

Downtime

1.92%

Com/Con

3.87%

Maintenance

18.43%

Holiday

2.48%

Interlock

0.75%

Injection

1.11%

	
 

 	 




		

	


	




		

	


		

 

	

 	



 	



 
	 		 	

 
	 		


     ! " 

#
$
 %!      "   

&

$
  ' '  ' '

(	
	  !   % "

)

	     %% %" !!

	 "!%     " 

*  !    ! !

	 %  %  ! % 

(

  !  !   % 

(
   "" ! %% %  !


+
  !  "   !

,
*
$
 % % "  %   !"

 "     


	



	 % ""   % " 

	

	



	




 7 - 1 Publications

The following pages list all publication citations 

reported to the NSLS in FY 2002 (October 1, 2001 

through September 30, 2002). Citations are listed in 

order of beamline number and then alphabetically by 

the last name of the first author. This list contains 

unique citations for journal, published conference 

proceedings, books, chapters in books, formal reports, 

informal reports, technical reports, theses, 

dissertations, and patents when reported. For citation 

submissions where research was performed on more 

than one beamline, the citation is listed under each 

beamline. However, each citation was only counted 

once. Citations bearing publication dates prior to the 

Year 2002 are listed only if they had not been 

previously reported to the NSLS and did not appear in 

a prior fiscal yearís activity report. Diligent effort has 

been made to ensure that each reference is unique and 

complete. For journal articles, online searches were 

performed to locate missing reference information 

(e.g., year of publication, volume, issue or page 

numbers). With regard to conference papers, 

considerable effort was put into ensuring that the 

citations appeared in published proceedings. Many 

citations for conferences papers have been omitted 

from this list if verification could not be made. We 

apologize to our users and authors for any citations 

incorrectly omitted. 

Several types of journal articles are reported in 

this list, including premiere journals, peer-reviewed 

journals and a few that are not peer-reviewed. 

Premiere journals include: Physical Review Letters, 

Science, Nature, Cell, EMBO Journal, Nature Structural 

Biology, Proceedings of the National Academy of 

Sciences of the United States of America, Structure, 

and Applied Physics Letters. 

In FY 2002, the following types and numbers of 

publication citations were reported to the NSLS where 

research was performed in part or in whole at the 

NSLS. 

Journals, peer-reviewed, premiere 134 

Journals, other peer-reviewed 437 

Journals, non peer-reviewed 22 

Total Journals and Magazines 593 

Books/Chapters in Books 14 

Published Conference Proceedings 79 

Reports: Technical, Formal, Informal 3 

Theses/Dissertations 19 

Patents 0 

Total Misc. Publications 115 

Total Citations Listed 708

NSLS VUV User Publications 69 

NSLS X-Ray User Publications 584 

NSLS Staff Publications 55 

 708

NSLS Users 

Beamline U1A

S Bent. Attaching Organic Layers to Semiconductor 

Surfaces. J. Phys. Chem. B. 106 (11), 2830-2842 

(2002). 

Q Du, N Carrasco, M Teplova, C Wilds, M Egli, Z Huang. 

Internal Derivatizatino of Oligonucleotides with 

Selenium for X-ray Crystallography using MAD. J. 

Am. Chem. Soc.. 124 (1), 24-25 (2002). 

G Haehner, R Hofer, I Klingenfuss. Order and 

Orientation in Self-Assembled Long Chain 

Alkanephosphate Monolayers. Langmuir. 17, 7047 

(2001). 

H Hwu, J Eng, Jr., J Chen. Ni/Pt(111) Bimetallic 

Surfaces: Unique Chemistry at Monolayer Ni 

Coverage. J. Am. Chem. Soc.. 124 (4), 702-709 

(2002). 

M Zwahlen, S Tosatti, M Textor, G Haehner. 

Orientation in Methyl- and Hydroxyl-Terminated SelfAssembled Alkanephosphate Monolayers on Titanium 

Oxide Surfaces Investigated with Soft X-ray 

Absorption. Langmuir. 18, 3957 (2002). 

Beamline U2A

R Angel, D Frost, N Ross, R Hemley. Stabilities and 

equations of state of dense hydrous magnesium 

silicates. Phys. Earth Planet. Interiors. 127, 181-196 

(2001). 

T Antsygina, K Chishko, Y Freiman, S Tretyak, R 

Hemley. Analytical approach to mean field theory of 

the BSP transition in solid hydrogens under pressure. 

J. Low Temp. Phys.. 122, 425-432 (2001). 

B Chen, D Muthu, Z Liu, A Sleigt, M Kruger. Highpressure Raman and infrared study of HfW2O8. Phys. 

Rev. B. 64, 214111 (2001). 

Y Freiman, S Tretyak, A Jezowski, R Hemley. Selfconsistent theory of lattice distortion in solid p-H2, oD2, and HD. J. Low Temp. Phys.. 122, 537-544 

(2001). 

A Goncharov, E Gregoryanz, R Hemley, H Mao. 

Spectroscopic studies of the vibrational and electronic 

properties of solid hydrogen to 285 GPa. Proc Natl 

Acad Sci USA. 98, 14234-14237 (2001). 

A Goncharov, E Gregoryanz, H Mao, R Hemley. 

Vibrational dynamics of solid molecular nitrogen to 

megabar pressures. Low Temp. Phys.. 27, 866 

(2001). 

D Klug, M Zgierski, J Tse, Z Liu, J Kincaid, K Czarnecki, 

R Hemley. Doming Modes and Dynamics of Model 

Heme Compounds. Proc Natl Acad Sci USA. 99 (20), 

12526-12530 (2002). 

M Koch-Mueller, Y Fei, E Hauri, Z Liu. Location and 

Quantitative Analysis of OH in Coesite. Phys. Chem. 

Miner.. 28, 693 (2001). 

M Koch-Mueller, A Hofmeister, Y Fei, Z Liu. Highpressure IR-spectra and the thermodynamic 

properties of chloritoid. Am. Mineral.. 87, 609-622 

(2002). 
Activity Report 2002 7 - 2 

Beamline U2B

R Huang, L Miller, C Carlson, M Chance. 

Characterization of Bone Mineral Compositon in the 

Proximal Tibia of Cynormolgus Monkeys: The Effect 

of Ovariectomy and Nandrolone Decanoate 

Treatment. Bone. 30, 492-497 (2002). 

R Huang. Bone Chemistry of Osteoporosis Revealed by 

Synchrotron Infrared Microspectroscopy . Ph.D. 

Thesis. Albert Einstein College of Medicine, Bronx . 

(2002). 

N Marinkovic, R Huang, P Bromberg, M Sullivan, E 

Sperber, S Moshe, L Miller, K Jones, E Chouparova, 

et al.. Center for Synchrotron Biosciences' U2B 

Beamline: An International Resource for Biological 

Infrared Spectroscopy. J. Synch. Rad.. 9, 189-197 

(2002). 

D Wetzel, G Williams. Localized (5 Ïm) Probing and 

Detailed Mapping of Hair with. Fourier Transform 

Spectroscopy, p. 302-305, American Institute of 

Physics, Woodbury. (1998). 

Beamline U4A

M Ulrich, R Johnson, J Hong, J Rowe, G Lucovsky, J 

Quinton, T Madey. Interface electronic structure of 

Ta2O5-Al2O3 alloys for Si-field-effect transistor gate 

dielectric applications. J. Vac. Sci. Technol., B. 20

(4), 1732-1738 (2002). 

Beamline U4B

A Vairavamurthy, S Wang. Organic Nitrogen in 

Geomacromolecules: Insights on Speciation and 

Transformation with K-edge XANES Spectroscopy. 

Environ. Sci. Tech.. 36 (14), 3050-3056 (2002). 

Beamline U4IR

P Brierley, B Badeau, P Dumas, M Smith, G Williams. 

Performance of a rapid-scan vacuum Michelson 

interferometer. Rev. Sci. Instrum.. 73 (3), 1595-

1598 (2002). 

P Dumas, M Hein, A Otto, B Persson, P Rudolf, R Raval, 

G Williams. Friction of Molecules on Metallic Surfaces: 

Experimental Approach using Synchrotron Infrared 

Spectroscopy. Surf. Sci.. 433-435, 797-805 (1999). 

K Nicholson. The Nature of Si-H Bonds in Model Device 

Interfaces. Ph.D. Thesis. University of Michigan, Ann 

Arbor. (2002). 

P Rudolf, R Raval, P Dumas, G Williams. Vibrational 

dynamics of fullerene molecules adsorbed on metal 

surfaces studied with synchrotron infrared radiation, 

invited paper. Appl. Phys. A. 75 (1), 147-153 (2002). 

Beamline U7A

D Abraham, R Twesten, M Balasubramanian, I Petrov, J 

McBreen, K Amine. Surface changes on 

LiNi0.8Co0.2O2 particles during testing of high-power 

lithium-ion cells. Electrochem. Commun.. 4, 620-625 

(2002). 

L Andruzzi, A Hexemer, X Li, C Ober, E Kramer, G Galli, 

E Chiellini. Surface Control Using Polymer Brushes 

Produced By Controlled Radical Polymerization. ACS 

Symp. Ser.. 43 (2), 76 (2002). 

T Baas, L Gamble, K Hauch, D Castner, T Sasaki. 

Characterization of a Cysteine-Containing Peptide 

Tether Immobilized onto a Gold Surface. Langmuir. 

18, 4898-4902 (2002). 

M Balasubramanian, H Lee, X Sun, X Yang, A 

Moodenbaugh, J McBreen, D Fisher, Z Fu. Formation 

of SEI on Cycled Lithium-Ion Battery Cathodes: Soft 

X-ray Absorption Study. Electrochem. Solid-State 

Lett.. 5 (1), A22-25 (2002). 

R Bhat, D Fischer, J Genzer. Fabricating Planar 

Nanoparticle Assemblies with Number Density 

Gradients. Langmuir. 18, 5640-5643 (2002). 

R Bubeck, J Li, P Dvornic, A Hexemer, X Li, L Andruzzi, 

D Fischer. NEXAFS of Poly(amidoamineorganosilicon) (PAMAMOS) Dendrimer Network 

Nanocomposites. American Physical Society, Vol 47, 

p. 210, (2002). 

Z Chang, Z Song, G Liu, J Rodriguez, J Hrbek. 

Synthesis, electronic and chemical properties of 

MoOx clusters on Au(111). Surf. Sci.. 512 (1-2), 

L353 (2002). 

K Efimenko, B Novick, R Carbonell, J DeSimone, J 

Genzer. Formation of Self-Assembled Monolayers of 

Semifluorinated and Hydrocarbon Chlorosilane 

Precursors on Silica Surfaces from Liquid Carbon 

Dioxide. Langmuir. 18, 6170-6179 (2002). 

K Efimenko, J Genzer. How to prepare tunable planar 

molecular chemical gradients. Advanced Materials. 

13, 1560 (2001). 

C Evans, A Smith, D Burnett, A Marsh, D Fischer, J 

Gland. Polymer Conversion Measurement of 

Diacetylene-Containing Thin Films and Monolayers 

Using Soft X-ray Fluorescence Spectroscopy. J. Phys. 

Chem. B. 106, 9036-9034 (2002). 

D Fischer, S Sambasivan, A Kuperman, Y Platonov , J 

Wood . Multilayer mirror fluorescence detection 

system for photon-in photon-out in-situ carbon Kedge NEXAFS . Synch. Rad. News. 15, 16-20 (2002). 

D Fischer, S Sambasivan, A Kuperman, Y Platonov , J 

Wood . Focusing Multilayer Mirror Detection System 

for Carbon K edge Soft X-ray Absorption 

Spectroscopy. Rev. Sci. Instrum.. 73, 1469-1475 

(2002). 

L Gamble, B Ravel, D Fischer, D Castner. Surface 

Structure and Orientation of PTFE Films Determined 

by Experimental and FEFF8-Calculated NEXAFS 

Spectra. Langmuir. 18 (6), 1963-1967 (2002). 

J Lenhart, E Lin, C Soles, R Jones, W Wu, D Fischer, S 

Sambasivan, D Goldfarb, M Angelopoulos. Probing 

Surface and Bulk Deprotection in Resist Films using 

NEXAFS. ACS Div. Poly. Mat.: Sci. and Eng, Vol 87, p. 

417, sponsored by American Chemical Society. 

(2002). 

X Li, L Andruzzi, E Chiellini, G Galli, C Ober, A 

Hexemer, E Kramer, D Fischer. Semifluorinated 

Aromatic Side-Chain Polystyrene-Based Block 

Copolymers: Bulk Structure and Surface Orientation 

Studies. Macromolecules. 35 (21), 8078 (2002). 

G Liu, J Rodriguez, J Dvorak, J Hrbek, T Jirsak. 

Chemistry of sulfur-containing molecules on Au(111): 

thiophene, sulfur dioxide, and methanethiol 

adsorption. Surf. Sci.. 505, 295-307 (2002). 
7 - 3 Publications

G Liu, J Rodriquez, Z Chang, J Hrbek, L Gonzalez. 

Adsorption of Methanethiol on Stoichiometric and 

Defective TiO2(110) Surfaces: A Combined 

Experimental and Theoretical Study. J. Phys. Chem. 

B. 106, 9883-9891 (2002). 

J Rodriguez, G Liu, T Jirsak, J Hrbek, Z Chang, J 

Dvorak, A Maiti. Activiation of Gold on Titania: 

Adsorption and Reaction of SO2 on Au/TiO2(110). J. 

Am. Chem. Soc.. 124 (18), 5242-5250 (2002). 

J Rodriguez. Electronic and chemical properties of 

palladium in bimetallic systems: How much do we 

know about heteronuclear metal-metal bonding?. The 

Chemical Physics of Solid Surfaces: Surface Alloys 

and Alloy Surfaces, p. 343, Elsevier, Amsterdam. 

(2002). 

J Rodriguez, J Hrbek, Z Chang, J Dvorak, T Jirsak, A 

Maiti. Importance of O vacancies in the behavior of 

oxide surfaces: Adsorption of Sulfur on TiO2(110). 

Phys. Rev. B. 65 (23), 235414 (2002). 

J Rodriguez. Environmental Catalysis and The 

Chemistry of SO2 on Oxide Surfaces. Ciencia. 9, 139 

(2001). 

J Rodriguez, J Hrbek. Interaction of sulphur with 

bimetallic surfaces: Effects of Structural, electronic 

and chemical properties. The Chemical Physics of 

Solid Surfaces: Surface Alloys and Alloy Surfaces, p. 

374, Elsevier, Amsterdam. (2002). 

J Rodriguez, T Jirsak, L Gonzalez, J Evans, M Perez, A 

Maiti. Reaction of SO2 with pure and metal-doped 

MgO: Basic principles for the cleavage of S-O bonds. 

J. Chem. Phys.. 115, 10914 (2001). 

T Wu, K Efimenko, J Genzer. Combinatorial Study of 

the Mushroom-to-brush crossover in surface 

anchored polyacrylamide. J. Am. Chem. Soc.. 124, 

9394 (2002). 

Z Yang, R Wu, J Rodriguez. First-Principles Study of the 

Adsorption of Sulfur on Pt(111): S Core-level Shifts 

and the Nature of the Pt-S Bond. Phys. Rev. B: 

Condens. Matter. 65, 155409 (2002). 

Y Zhu, A Moodenbaugh, G Schneider, J Davenport, T 

Vogt, Q Li, G Gu, D Fischer, J Tafto. Unraveling the 

Symmetry of the Hole States near the Fermi Level in 

the MgB2 Superconductor. Phys. Rev. Lett.. 88 (24), 

247002-1 (2002). 

Beamline U7B

S Park, H Gies, B Toby, J Parise. Characterization of a 

New Microporous Lithozincosilicate with ANA 

Topology. Chem. Mater.. 14, 3187-3196 (2002). 

Beamline U8B

K Miller, C John, K Zhang, K Nicholson, F McFeely, M 

Banaszak Holl. Self-limiting chemical vapor 

deposition of an ultra-thin silicon oxide film using tri-

(tert-butoxy)silanol. Thin Solid Films. 397 (1-2), 78-

82 (2001). 

K Nicholson. The Nature of Si-H Bonds in Model Device 

Interfaces. Ph.D. Thesis. University of Michigan, Ann 

Arbor. (2002). 

K Nicholson, K Zhang, M Banaszak Holl, F McFeely, G 

Calzaferri, U Pernisz. Formation of Mixed Layers 

Derived from Functional Silicon Oxide Clusters on 

Gold. Langmuir. 17 (25), 7879-7885 (2001). 

T Owens, K Nicholson, M Banaszak Holl, S S ̧zer. 

Formation of Alkylsilane based Monolayers on Gold. J. 

Am. Chem. Soc.. 124 (24), 6800-6801 (2002). 

S Sayan, E Garfunkel, S Suzer. Soft x-ray 

photoemission studies of the HfO2/SiO2/Si system. 

Appl. Phys. Lett.. 80 (12), 2135-2137 (2002). 

K Schneider, T Owens, K Nicholson, B Ludwig, J 

Greeley, B Orr, M Banaszak Holl. Investigation of 

Hydridosilsesquioxane-Based Silicon Oxide Deposition 

on Si(111)-7×7. Langmuir. 18 (16), 6233-6241 

(2002). 

Beamline U9B

M Baniecki, W Mcgrath, S Mcwhirter, C Li, D Toledo, P 

Pellicena, D Barnard, K Thorn, W Mangel. Interaction 

of the human adenovirus proteinase with its 11-

amino acid cofactor pVIc. Biochemistry. 40, 12349-

56 (2001). 

J Sutherland. Simultaneous measurement of circular 

dichroism and fluorescence polarization anisotropy. 

Clinical Diagnostic Systems: Technologies and 

Instrumentation, Vol 4625, p. 126-136, sponsored by 

Proceedings of SPIE. (2002). 

Beamline U10A

J Tu, G Carr, V Perebeinos. Optical Properties of c-Axis 

Oriented Superconducting MgB2 Films. Phys. Rev. 

Lett.. 87, 277001 (2001). 

Beamline U10B

M Jaime Vasquez, G Halada, C Calyton, J Longtin. On 

the Nature of the Chromate Conversion Coating 

Formed on Intermetallic Constituents of AA2024-T3. 

Surf. Interface Anal.. 33 (7), 607-616 (2001). 

M Jaime Vasquez, G Halada, C Clayton. The Application 

of Synchrotron-based Spectroscopic Techniques to 

the Study of Chromate Conversion Coatings. 

Electrochim. Acta. 47 (19), 3105-3115 (2002). 

L Keller, S Hony, J Bradley, F Molster, L Waters, J 

Bouwman, A deKoter, D Brownlee, G Flynn, et al.. 

Identification of Iron Sulphide Grains in 

Protoplanetary Disks. Nature. 417, 148-150 (2002). 

L Kreplak, F Briki, Y Duvault, J Doucet, C Merigoux, F 

Leroy, J Leveque, L Miller, G Carr, et al.. Profiling 

lipids across Caucasian and African-American hair 

transverse cuts, using synchrotron infrared 

microspectrometry. Int. J. Cosmetic Sci.. 23 (6), 

369-374 (2001). 

J Tetenbaum, L Miller. A new spectroscopic approach to 

examining the role of disulfide bonds in the Structure 

and Unfolding of Soybean Trypsin Inhibitor. 

Biochemistry. 40, 12215-19 (2001). 

M Vasquez, G Halada, C Clayton, J Longtin. 

Composition of Surface Treated Thin Films Analogs of 

Intermetallic Constituents in AA2024-T3. Corrosion 

and Corrosion Prevention of Low Density Metal and 

Alloys, Vol PV2000-23, p. 57-68, sponsored by The 

Electrochemical Society. (2001). 
Activity Report 2002 7 - 4 

M Vasquez, G Halada, C Clayton. Composition of 

Chromate Conversion Coatings Formed on 

multilayered Thin Films of AA2024-T3 matrix and 

Al2Cu, Al2CuMg and Al20Cu2(FeMn).. Vol PV2001-

22, p. 444-453, (2001). 

Beamline U12A

D Mullins, S Overbury. Coverage Dependent 

Dissociation of NO on Rh Supported on Cerium Oxide 

Thin Films. Surf. Sci.. 511, L293 - L297 (2002). 

D Mullins, K Zhang. Metal - Support Interactions 

between Pt and Thin Film Cerium Oxide. Surf. Sci.. 

513, 163 - 173 (2002). 

Beamline U12B

P Cebe, G Georgiev, P Dai, M Capel. Structural Studies 

of Polymers Using Small Angle X-ray Scattering and 

Optical Ellipsometry. Proceedings of the American 

Crystallographic Association, p. 70, (2001). 

P Cebe, P Dai, G Georgiev, B Feinberg, N Gilfoy. X-ray 

diffraction and optical ellipsometry: Complementary 

techniques for study of polymer structure. Poly ACS, 

Polymer Preprints, Vol 43, (2001). 

Beamline U12IR

S Kramer. Direct Observation of Beam Impedance 

Above Cut-off. Phys. Rev. ST AB. 5, 112001-1 

(2002). 

R Lobo, J LaVeigne, D Reitze. Subnanosecond, timeresolved, broadband infrared spectroscopy using 

synchrotron radiation. Rev. Sci. Instrum.. 73 (1), 1 

(2002). 

Beamline U13UB

A Fedorov, T Valla, F Liu, P Johnson, M Weinert, P 

Allen. Spin-Resolved Photoemission Study of 

Photohole Lifetimes in Ferromagnetic Gadolinium. 

Phys. Rev. B. 65, 212409 (2002). 

T Valla, P Johnson, Z Yusof, B Wells, Q Li, S Loureiro, R 

Cava, M Mikami, Y Mori, et al.. CoherenceIncoherence and Dimensional Crossover in Layered 

Strongly Correlated Metals. Nature. 417, 627-630 

(2002). 

Z Yusof, B Wells, T Valla, A Fedorov, P Johnson, Q Li, C 

Kendziora, S Jian, D Hinks. Quasiparticle Liquid in 

Highly Overdoped Bi2Sr2CaCu2O8+delta. Phys. Rev. 

Lett.. 88 (16), 167006 (2002). 

Beamline U16B

M Butterfield, R Bartynski, S Hulbert. Pd M45VV Auguer 

Spectrum Determined by Auger-Photoelectron 

Coincidence Spectroscopy: Intrinsic Line Shape and 

Coster-Kronig Transitions. Phys. Rev. B. 66, 115115 

(2002). 

Beamline X1A1

M Carlucci-Dayton. Nomarski Differential Phase 

Contrast Using a Scanning Transmission X-ray 

Microscope. MSI Thesis. Dept. Physics & Astronomy, 

SUNY Stony Brook, Stony Brook. (2000). 

F Claret, A Bauer, T Schaefer, L Griffault, B Lanson. 

Experimental investigation of the interaction of clays 

with high pH solutions: A case study from the future 

French underground laboratory. Clays and Clay 

Minerals. 50, 632-645 (2002). 

T Coffey, S Urquhart, H Ade. Characterization of the 

Effects of Soft X-ray Irradiation on Polymers. J. 

Electron. Spectrosc. Relat. Phenom.. 122 (1), 65-78 

(2002). 

M Feser. Scanning Transmission X-ray Microscopy With 

a Segmented Detector. Ph.D. Thesis. SUNY Stony 

Brook, Stony Brook. (2002). 

A Hitchcock, I Koprinarov, T Tyliszczak, E Rightor, G 

Mitchell, M Dineen, F Hayes, W Lidy, R Priester, et al. 

Optimization of scanning transmission X-ray 

microscopy for the identification and quantitation of 

reinforcing particles in polyurethanes. 

Ultramicroscopy. 88 (1), 33-49 (2001). 

A Kalukin, B Winn, Y Wang, C Jacobsen, Z Levine, J Fu. 

Calibration of high-resolution X-ray tomography with 

atomic force microscopy. J. Res - NIST. 105 (6), 

867-874 (2000). 

K Kaznacheyev, A Osana, C Jacobsen, O Plashkevych, 

O Vahtras, H Agren, V Carravetta, A Hitchcock. 

Innershell absorption Spectroscopy of amino acids. J. 

Phys. Chem. A. 106 (13), 3153-3168 (2002). 

G Mitchell, L Wilson, M Dineen, S Urquhart, F Hayes, E 

Rightor, P Hitchcock, H Ade. Quantitative 

Characterization of Microscopic Variations in the 

Cross-Link Density of Gels. Macromolecules. 35 (4), 

1336-1341 (2002). 

A Osanna. Soft x-ray spectromicroscopy in a cryo 

scanning transmission x-ray microscope. Ph.D. 

Thesis. Dept. Physics & Astronomy, SUNY Stony 

Brook, Stony Brook. (2000). 

M Plaschke, J Rothe, T Schaefer, M Denecke, K 

Dardenne, S Pompe, K Heise. Combined AFM and 

STXM in situ study of the influence of Eu(III) on the 

agglomeration of humic acid. Coll. Surf. A. 197 (1-

3), 245-256 (2002). 

E Rightor, S Urquhart, A Hitchcock, H Ade, A Smith, G 

Mitchell, R Priester, A Aneja, G Appel, et al. 

Identification and Quantitation of Urea Precipitates in 

Flexible Polyurethane Foam Formulations by X-ray 

Spectromicroscopy. Macromolecules. 35, 5873-5882 

(2002). 

A Scheinost, R Kretzschmar, I Christl, C Jacobsen. 

Carbon group chemistry of humic and fulvic acid: A 

comparison of C-1s NEXAFS and 13C-NMR 

spectroscopies. Humic Substances: Structures, 

Models and Functions, p. 37-45, Royal Society of 

Chemistry, Cambridge. (2001). 

A Smith, S Urquhart, D Winesett, G Mitchell, H Ade. 

Use of near edge X-ray absorption fine structure 

spectromicroscopy to characterize multicomponent 

polymeric systems. Appl Spectrosc. 55 (12), 1676-

1681 (2001). 
7 - 5 Publications

Y Wang. Three-dimensional imaging in soft x-ray 

microscopy. Ph.D. Thesis. Dept. Physics & 

Astronomy, SUNY Stony Brook, Stony Brook. (1998). 

Y Zhang, S Ge, B Tang, T Koga, M Rafailovich, J 

Sokolov, D Peiffer, Z Li, A Dias, et al. Effect of carbon 

black and silica fillers in elastomer blends. 

Macromolecules. 34 (20), 7056-7065 (2001). 

Beamline X1B

P Abbamonte, L Venema, A Rusydi, G Logvenov, I 

Bozovic, G Sawatzky. A Structural Probe of the 

Doped Holes in Cuprates Superconductors. Science. 

297, 581-584 (2002). 

E Rennie, U Hergenhahn, O Kugeler, A R ̧del, S 

Marburger, A Bradshaw. A Core-Level Photoionization 

Study of Furan. J. Chem. Phys.. 117 (14), 6524-

6532 (2002). 

P Ryan, C McGuinness, J Downes, K Smith, D 

Doppalapudi, T Moustakas. Band-gap evolution, 

hybridization and thermal stability of In1-xGaxN 

alloys studied by soft x-ray emission and absorption. 

Phys. Rev. B. 65 (20), 5201 (2002). 

T Schitt, L Duda, A Augustsson, J Guo, J Nordgren, J 

Downes, C McGuinness, K Smith, G Dhalenne, et al. 

Resonant soft x-ray emission spectroscopy of V2O3, 

VO2 and NaV2O5. Surf. Rev. Lett.. 9 (2), 1369-1374 

(2002). 

Beamline X2B

G Wu, B Rodrigues, P Coppens. The correction of 

reflection intensities for incomplete absorption of high 

energy X-rays in the CCD phosphor. J. Appl. Cryst.. 

35, 356-359 (2002). 

Beamline X3A1

C Kim, S Pillet, G Wu, W Fullagar, P Coppens. Excited 

state structure by time-resolved X-ray diffraction. 

Acta Cryst. A. 58, 133-137 (2002). 

T Koritsanszky, P Coppens. Chemical applications of Xray charge density analysis. Chem. Rev.. 101, 1583-

1628 (2001). 

X Li, G Wu, Y Abramov, A Volkov, P Coppens. 

Application of charge density methods to a protein 

model compound: calculation of coulombic 

intermolecular interaction energies from the 

experimental charge density. Proc Natl Acad Sci USA. 

99 (19), 12132-12137 (2002). 

G Wu, B Rodrigues, P Coppens. The correction of 

reflection intensities for incomplete absorption of high 

energy X-rays in the CCD phosphor. J. Appl. Cryst.. 

35, 356-359 (2002). 

Beamline X3A2

M Gelfer, A Waddon, K Schmidt-Rohr, R Gale, L 

Kleiner, R Bergren. Annealing_induced Increase of 

Permeability and Amophous-Phase Mobility in 

Ethylene-Vinylacetate Copolymer. J. Polym. Sci., Part 

B: Polym. Phys.. 39, 2774-2779 (2002). 

S Ran, X Zong, D Fang, B Hsiao, B Chu, P Cunniff, R 

Phillips. Studies of the mesophase development in 

polymeric fibers during deformation by synchrotron 

SAXS/WAXD. J. Mater. Sci.. 36, 3071-3077 (2001). 

R Seright, J Liang, B Lindquist, J Dunsmuir. 

Characterizing Disproportionate Permeability 

Reduction Using Synchrotron X-Ray Computed 

Microtomography. Soc. Petrol. Eng. J. Reservior 

Evaluation and Engineering. 5 (5), 355-364 (2002). 

Beamline X3B1

D Balzar, H Ledbetter, P Stephens, E Park, J Routbort. 

Dislocation-density changes upon poling of 

polycrystalline BaTiO3. Phys. Rev. B. 59, 3414-3420 

(1999). 

D Bohle, A Kosar, P Stephens. Phase homogeneity and 

crystal morphology of the malaria pigment betahematin. Acta Cryst. D. 58, 1752-1756 (2002). 

C Botez, W Elliot, P Miceli, P Stephens. Vacancy 

formation in homoepitaxially grown Ag films and its 

effect on surface morphology. Phys. Rev. B. 66, 

075418 (2002). 

M Bushey, A Hwang, P Stephens, C Nuckolls. The 

consequences of chirality in crowded arenes - 

Macromolecular helicity, hierarchical ordering, and 

directed assembly. Angew. Chem. Int. Ed.. 41, 2828-

2831 (2002). 

R Dinnebier, S Vensky, M Jansen, P Stephens. The First 

Crystallographic Proof of the Peroxodicarbonate Anion 

in K2[C2O6] from Powder Diffraction Data. Z. 

Kristallogr.. 19 (Suppl. Issue), 42 (2002). 

R Dinnebier, S Jelonek, J Sieler, P Stephens. The solid 

state structures of K salicylate and Rb salicylate by 

high resolution X-ray powder diffraction. Z. Anorg. 

Allg. Chem.. 628 (2), 363-368 (2001). 

R Dinnebier, H Lerner, L Ding, K Shankland, W David, P 

Stephens, M Wagner. One-Dimensional Spin Chains 

from CuII Ions and 2,5-Bis(pyrazol-1-yl)-1,4-

dihydroxybenzene. Z. Anorg. Allg. Chem.. 628 (1), 

310-314 (2002). 

R Dinnebier, L Ding, K Mab, M Neumann, N Tanpipat, F 

Leusen, P Stephens, M Wagner. Crystal Structure of a 

Rigid Ferrocene-based Macrocycle from High 

Resolution X-ray Powder Diffraction.. 

Organometallics. 20, 5642-5647 (2001). 

R Dinnebier, O Gunnarsson, H Brumm, E Koch, P 

Stephens, A Huq, M Jansen. Structure of Haloform 

Intercalated C60 and its Influence on 

Superconductive Properties. Science. 296, 109-113 

(2002). 

R Dinnebier, S Vensky, P Stephens, M Jansen. Crystal 

Structure of K2[C2O6] - First Proof of existence and 

Constitution of a Peroxodicarbonate Ion. Angew. 

Chem. Int. Ed.. 41 (11), 1922-1924 (2002). 

A Hoennerscheid, R Dinnebier, M Jansen. Reversible 

Dimerization of C60 molecules in the Crystal 

Structure of Bis(arene)chromium Fulleride 

Cr(C7H8)2C60. Acta Cryst. B. B58, 482-488 (2002). 

A Huq, P Stephens, G Bendele, R Ibberson. Polymeric 

fullerene chains in RbC60 and KC60. Chem. Phys. 

Lett.. 347, 13-22 (2001). 
Activity Report 2002 7 - 6 

J Kaduk. Terephthalate salts of dipositive cations. Acta 

Cryst. B. 58, 815-822 (2002). 

P Karen, P Woodward, P Santosh, T Vogt, P Stephens, 

S Pagola. Verwey transition under oxygen loading in 

RBaFe2O5+w (R=Nd and Sm). J. Solid State Chem.. 

167, 480-493 (2002). 

G Kioseoglou, S Kim, Y Soo, X Chen, H Luo, Y Kao, Y 

Sasaki, X Liu, J Furdyna. Investigation of nanoscale 

structure in digital layers of Mn/GaAs and MnGa/GaAs 

. Appl. Phys. Lett.. 80, 1150 (2002). 

H Kisch, B Eisen, R Dinnebier, K Shankland, W David, F 

Knoch. Chiral Metal Dithiolene - Viologen Ion Pairs - 

Synthesis and Electrical Conductivity. Chem. Eur. J.. 

7 (3), 738-748 (2001). 

M Nyman, A Tripathi, J Parise, R Maxwell, T Nenoff. 

Sandia Octahedral Molecular Sieves (SOMS): 

Structural and Property Effects of Charge-Balancing 

the MIV-Substituted (M = Ti, Zr) Niobate Framework. 

J. Am. Chem. Soc.. 124 (8), 1704-1713 (2002). 

S Schlecht, R Dinnebier, K Friese. Mild Direct Synthesis 

of Organofunctionalized Alkyltin Bromides 

[X?(CH2)n?]2SnBr2 (X=Cl,CN, COOCH3; n=2-4) 

from the Activated Element ñ Crystal Structure of 

(H3COOCC2H4)2SnBr2. Z. Anorg. Allg. Chem.. 628

(4), 725-727 (2002). 

Y Soo, G Kioseoglou, S Kim, Y Kao, P Sujatha Devi, J 

Parise, R Gambino, P Gouma. Local Environment 

Surrounding Magnetic Impurity Atoms in a Structural 

Phase Transition of Co-Doped TiO2 Nanocrystal 

Ferromagnetic Semiconductors. Appl. Phys. Lett.. 81, 

655-657 (2002). 

Y Soo, G Kioseoglou, S Kim, X Chen, H Luo, Y Kao, Y 

Sasaki, X Liu, J Furdyna. Studies of Mn/GaAs Digital 

Alloys Using X-ray Absorption Fine Structure and Xray. Appl. Phys. Lett.. 80, 2654 (2002). 

P Stephens, D Cox. Structure solution from powder 

diffraction at the National Synchrotron Light Source. 

Brookhaven National Laboratory, Upton. Prepared for 

U.S. Department of Energy. (1998). 

P Stephens, D Cox, A Fitch. Synchrotron radiation 

powder diffraction. Structure Determination by 

Powder Diffraction, p. 49-87, Oxford University Press, 

Oxford. (2002). 

P Stephens. Phenomenological model of anisotropic 

peak broadening in powder diffraction. J. Appl. 

Cryst.. 32, 281-289 (1999). 

C Tedesco, R Dinnebier, F Olbrich, S van Smaalen. The 

Disordered Crystal Structure of 

Pentamethylcyclopentadienylsodum NaCp* as seen 

by High Resolution X-ray Powder Diffraction. Acta 

Cryst. B. 57, 673-679 (2001). 

A Vecchione, M Gombos, S Pace, L Marchese, G 

Cerrato, C Tedesco, P Stephens, C Noce. Crystal 

structure and morphology of the NdSr2RuCu2Oy 

compound. Eur. Phys. J. B. 26, 51-55 (2002). 

R von Dreele. Combined Rietveld and stereochemical 

restraint refinement of a protein crystal structure. J. 

Appl. Cryst.. 32, 1084-1089 (1999). 

R von Dreele. Binding of n-acetylglucosamine to 

Chicken Egg Lysozyme: A Powder Diffraction Study. 

Acta Cryst. D. 57, 1836-1842 (2001). 

Beamline X4A

N Armstrong, E Gouaux. Mechanisms for Activation and 

Antagonism of an AMPA-Sensitive Glutamate 

Receptor: Crystal Structures of the GluR2 Ligand 

Binding Core. Neuron. 28, 165-181 (2000). 

J Arndt, B Hao, V Ramakrishnan, T Cheng, M Chan. 

Crystal Structure of Novel Carboxypeptidase from the 

Hyperthermophilic Archaeon Pyrococcus furiosus. 

Structure. 10, 41-50 (2002). 

R Batra, R Khayat, L Tong. Molecular mechanism for 

dimerization to regulate the catalytic activity of 

human cytomegalovirus protease. Nat. Struct. Biol.. 

8, 810-817 (2001). 

V Bernier-Villamor, D Sampson, M Matunis, C Lima. 

Structural Basis for E2-Medicated SUMO Conjugation 

Revealed by a Complex Between UbiquitinConjugating Enzyme Ubc9 and RanGAP1. Cell. 108, 

345-356 (2002). 

T Boggon, J Murray, S Chappuis-Flament, E Wong, B 

Gumbiner, L Shapiro. C-Cadherin Ectodomain 

Structure and Implications for Cell Adhesion 

Mechanisms . Science. 296 (5571), 1308-1313 

(2002). 

R Bryk, C Lima, H Erdjument-Bromage, P Tempst, C 

Nathan. Metabolic Enzymes of Mycobacteria Linked to 

Antioxidant Defense by a Thioredoxin-Like Protein. 

Science. 295, 1073-1077 (2002). 

J Buglino, V Shen, P Hakimian, C Lima. Structural and 

Biochemical Analysis of the Obg GTP Binding Protein. 

Structure. 10, 51-62 (2002). 

S Charnock, I Brown, J Turkenburg, G Black, G Davies. 

Convergent Evolution Sheds Light on the Anti-betaElimination Mechanism Common to Family 1 and 10 

Polysaccharide Lyases. Proc Natl Acad Sci USA. 99

(19), 12067-12072 (2002). 

T Chiu, C Sohn, R Dickerson, R Johnson. Testing 

Water-mediated DNA Recognition by the Hin 

Recombinase. EMBO J.. 21, 801-814 (2002). 

H Cho, D Leahy. Structure of the extracellular region of 

HER3 reveals an interdomain tether. Science. 297, 

1330-3 (2002). 

C Dann, J Hsieh, A Rattner, D Sharma, J Nathans, D 

Leahy. Insights into Wnt binding and signaling from 

the structure of two Frizzled cysteine-rich domains. 

Nature. 412, 86-90 (2001). 

S Favelyukis, J Till, S Hubbard, W Miller. Structure and 

autoregulation of the insulin-like growth factor 1 

receptor kinase. Nat. Struct. Biol.. 8 (12), 1058-1063 

(2001). 

A Ferguson, R Chakraborty, B Smith, L Esser, D van 

der Helm, J Deisenhofer. Structural basis of gating by 

the outer membrane transporter FecA. Science. 295, 

1715-1719 (2002). 

C Garvie, J Hagman, C Wolberger. Structural Studies of 

Ets-1/Pax5 Complex Formation on DNA. Mol. Cell. 8

(6), 1267-1276 (2001). 

K Hakansson, C Miller. Structure of peptidase T from 

Salmonella typhimurium. Eur. J. Biochem.. 269 (2), 

443-50 (2002). 

B Hao, C Isaza, J Arndt, M Soltis, M Chan. Structurebased mechanism of O2 sensing and ligand 

discrimination by the FixL heme domain of 

Bradyrhizobium japonicum. Biochemistry. 41 (43), 

12952-8 (2002). 
7 - 7 Publications

B Hao, W Gong, T Ferguson, C James, J Krzycki, M 

Chan. A new UAG-encoded residue in the structure of 

a methanogen methyltransferase. Science. 296, 

1462 (2002). 

D Ho, G Coburn, Y Kang, B Cullen, M Georgiadis. The 

Crystal Structure and Mutational Analysis of a Novel 

RNA-Binding Domain Found in the Human Tap 

Nuclear mRNA Export Factor. Proc Natl Acad Sci USA. 

99, 1888-1893 (2002). 

A Hogner, J Kastrup, R Jin, T Liljefors, M Mayer, J 

Egebjerg, I Larsen, E Gouaux. Structural Basis of 

AMPA Receptor Activation and Ligand Selectivity. J. 

Mol. Biol.. 322, 93-109 (2002). 

J Hunt, S Weinkauf, L Henry, J Fak, P McNicholas, D 

Oliver, J Deisenhofer. Nucleotide Control of 

Interdomain Interactions in the Conformational 

Reaction Cycle of SecA. Science. 297, 2018-2026 

(2002). 

G Jogl, Y Shen, D Gebauer, J Li, K Wiegmann, H 

Kashkar, M Kronke, L Tong. Crystal Structure of the 

BEACH Domain Reveals an Unusual Fold and 

Extensive Association with a Novel PH Domain. EMBO 

J.. 21 (18), 4785-4795 (2002). 

J Keift, K Zhou, A Grech, R Jubin, J Doudna. Crystal 

Structure of an RNA Tertiary Domain Essential to HCV 

IRES-Mediated Translation Initiation. Nat. Struct. 

Biol.. 9, 370-374 (2002). 

R Khayat, R Batra, M Massariol, L Lagace, L Tong. 

Investigating the role of histidine 157 in the catalytic 

activity of human cytomegalovirus protease. 

Biochemistry. 40, 6344-6351 (2001). 

M Kumar, M Carson, M Hussain, H Krishna. Structures 

of Apolipoprotein A-II and a Lipid-Surrogate Complex 

Provide INsights into Apolipoprotein-Lipid 

Interactions. Biochemistry. 41, 11681-11691 (2002). 

C Lima. Analysis of the E. coli NifS CsdB Protein at 2.0A 

Reveals the Structural Basis for Perselenide and 

Persulfide Intermediate Formation. J. Mol. Biol.. 315, 

1199-1208 (2002). 

M Marino, M Banerjee, R Jonquieres, P Cossart, P 

Ghosh. GW domains of the L. monocytogenes 

invasion protein InlB are SH3-like and mediate 

binding to host ligands. EMBO J.. 21, 5623-5634 

(2002). 

S Patenaude, N Seto, S Borisova, A Szpacenko, S 

Marcus, M Palcic, S Evans. The Structural Basis for 

Specificity in Human ABO(H) Blood Group 

Biosynthesis. Nat. Struct. Biol.. 9 (9), 685-690 

(2002). 

Y Sun, R Olson, M Horning, N Armstrong, M Mayer, E 

Gouaux. Mechanism of Glutamate Receptor 

Desensitization. Nature. 417, 245-253 (2002). 

J Truglio, K Theis, S Leimkuhler, R Rappa, K 

Rajagopalan, C Kisker. Crystal Structures of the 

Active and Alloxanthine-Inhibited Forms of Xanthine 

Dehydrogenase from Rhodobacter capsulatus. 

Structure. 10 (1), 115-125 (2002). 

H Yang, P Jeffrey, J Miller, E Kinnucan, Y Sun, N 

Thoma, N Zheng, P Chen, N Zheng, et al. BRCA2 

Function in DNA Binding and Recombination from a 

BRCA2-DSS1-ssDNA Structure. Science. 297, 1837-

1848 (2002). 

H Ye, J Arron, B Lamothe, M Cirilli, T Kobayashi, N 

Shevde, D Segal, O Dzivenu, M Volgododskaia, et al.. 

Distinct molecular mechanism for initiating TRAF6 

signalling.. Nature. 418, 443-7 (2002). 

R Zhao, E Collins, R Bourret, R Silversmith. Structure 

and Catalytic Mechanism of the E. Coli Chemotaxis 

Phosphatase CheZ. Nat. Struct. Biol.. 9 (8), 570-575 

(2002). 

X Zhao, S Ghaffari, H Lodish, V Malashkevich, P Kim. 

Structure of the Bcr-Abl Oncoprotein Oligomerization 

Domain. Nat. Struct. Biol.. 9, 117-120 (2002). 

N Zheng, B Schulman, L Song, J Miller, P Jeffrey, P 

Wang, C Chu, D Koepp, S Elledge, et al. Structure of 

the Cul1-Rbx1-Skp1-F boxSkp2 SCF ubiquitin ligase 

complex. Nature. 416, 703-709 (2002). 

Beamline X5A

K Hicks, K Ardashev, M Blecher, A Caracappa, A 

Cichocki, C Commeaux, A D'Angelo, J Dideliz, R 

Deininger, et al.. Neutral pion production from 

deuterium at the LEGS facility. Int'l symposium on 

electromagnetic interactions in nuclear and hadron 

physics, Vol 2001, (2001). 

M Lowry, F Lincoln, L Miceli, T Saitoh, A Sandorfi, X 

Wei, C Whisnant. Progress on the LEGS polarized HD 

target. Int'l workshop on polarized beams and 

polarized targets, PST 2001, Vol Sept 2001, (2001). 

A Sandorfi, G Blanpied, M Blecher, A Caracappa, C 

Djalali, G Giordano, K Hicks, S Hobliet, M Khandaker, 

et al.. Pion production and Compton scattering at 

LEGS. Proceedings NSTAR'2000, Vol Feb 16-17, 

(2000). 

C Whisnant, K Ardashev, V Bellini, M Blecher, C 

Cacace, A Caracappa, A Cichocki, C Commeaux, I 

Danchev, et al.. The first pion photoproduction 

results from polarized HD at LEGS. Int'l Symposium 

on Electromagnetic Interactions in Nuclear and 

Hadron Physics, Vol Dec 2001, p. N/A, sponsored by 

N/A. (2001). 

S Whisnant, K Ardashev, O Bartalini, M Blecher, A 

Caracappa, A D'Angelo, J Dideliz, R Deininger, K 

Hicks, et al.. The polarized HD ice target at LEGS. 

The symposium on the Gerasimov-Drell-Hearn sum 

rule and the spin structure in the resonance region, 

Vol June 2000, (2000). 

Beamline X6A

S Knight, D Choudhury, S Hultgren, J Pinkner, V 

Stojanoff, A Thompson. Structure of S Pilus 

Periplasmic Chaperone SfaE at 2.2 Å Resolution. Acta 

Cryst. D. 58, 1016-1022 (2002). 

Beamline X7A

B Bursten, M Chisholm, R Clark, S Firth, C Hadad, A 

MacIntosh, P Wilson, P Woodward, J Zaleski. OxalateBridged Complexes of Dimolybdenum and Ditungsten 

Supported by Pivalate Ligands: (tBuCO2)3M2(μO2CCO2)M2(O2CtBu)3. Correlation of the SolidState, Molecular, and Electronic Spectral Data. J. Am. 

Chem. Soc.. 124 (12), 3050-3063 (2002). 
Activity Report 2002 7 - 8 

N Hyatt, J Hriljac, Y Miyazaki, A Jephcoat, I Gameson, 

P Edwards. A Study of Structure-Compressibility 

Relationships in Layered Cuprate Materials. Phys. 

Rev. B. 65, 014507 (2002). 

B Kennedy, T Vogt, C Martin, J Parise, J Hriljac. 

Pressure-Induced Phase Transition in PrAlO3. Chem. 

Mater.. 14, 2644-2648 (2002). 

D La-Orauttapong, B Noheda, Z Ye, P Gehring, J 

Toulouse, D Cox, G Shirane. New phase diagram of 

relaxor ferroelectric (1-x)PbZn1/3Nb2/3O3-xPbTiO3. 

Phys. Rev. ST AB. 65, 144101 (2002). 

Y Lee, T Vogt, J Hriljac, J Parise, G Artioli. PressureInduced Volume Expansion of Zeolites in the Natrolite 

Family. J. Am. Chem. Soc.. 124 (19), 5466-5475 

(2002). 

Y Lee, T Vogt, J Hriljac, J Parise. Discovery of a 

Rhombohedral Form of the Li-Exhanged 

Aluminogermanate Zeolite RHO and its PressureTemperature-, and Composition-Induced Phase 

Transitions. Chem. Mater.. 14, 3501-3508 (2002). 

Y Lee, T Vogt, J Hriljac, J Parise, G Artioli. First 

Structural Investigation of a Super-hydrated Zeolite. 

J. Am. Chem. Soc.. 123, 12732-12733 (2001). 

Y Lee, J Hriljac, T Vogt, J Parise, M Edmondson, P 

Anderson, D Corbin, T Nagai. Phase Transition of 

Zeolite Rho at High-Pressure. J. Am. Chem. Soc.. 

123, 8418-8419 (2001). 

A Moodenbaugh, M Suenaga, L Lewis, D Cox, M Rupich, 

G Riley, Q Li, R Parrella. Superconducting Critical 

Current Densities and Synchrotron X-ray Diffraction 

Measurements of (Bi,Pb)(2)Sr(2)Ca(2)Cu(3)O(y)/Ag 

Composites. Physica C. 377 (1-2), 67-74 (2002). 

V Petkov, P Trikalitis, E Bozin, S Billinge, T Vogt, M 

Kanatzidis. Structure of V2O5·nH2O Xerogel Solved 

by the Atomic Pair Distribution Function Technique. J. 

Am. Chem. Soc.. 124, 10157-10162 (2002). 

G Wu, M Deem, S Elomari, R Medrud, T Maesen, C 

Kibby, C Chen, I Chan. Synthesis and Structure 

Determination by ZEFSAII of SSZ-55: A New HighSilica, Large-Pore Zeolite. J. Phys. Chem. B. 106 (2), 

264-270 (2002). 

Y Zhao, F Chu, R Von Dreele, Q Zhu. Structural Phase 

Transitions and Crystal Chemistry of HfV2 at Low 

Temperatures. Acta Cryst. B. 56, 601-6 (2000). 

Beamline X7B

K Barkigia, P Battioni, V Riou, D Mansuy, J Fajer. 

Supramolecular self-assembly of a fluorinated Zn 

porphyrin. Molecular structure of a two-dimensional 

network of amine-functionalized hexacoordinated Zn 

porphyrins. Chem. Commun.. (9), 956-957 (2002). 

K Barkigia, M Palacio, Y Sun, M Nogues, M Renner, F 

Varret, P Battioni, D Mansuy, I Fajer. Air-stable, 

electron-deficient fe(II) catalytic porphyrins. 

characterization and molecular structures of rare high 

spin fe(II)hexacoordinated porphyrins. Inorg. Chem.. 

41, 5647-5649 (2002). 

T Cheng, D Szalda, R Bullock. An Uncommon Bonding 

Mode of a Familiar Ligand: A Molybdenum Complex 

with a Four-Electron Donor Chelating N^3-PPh3 

LIgand and Its Structural Determination using 

Synchrotron Radiation. Chem. Commun.. 1999, 

1629-1630 (1999). 

M Ciraolo, J Hanson, B Toby, C Grey. combined X-ray 

and Neutron Powder Refinement and NMR Study of 

Hydrochlorofluorocarbon HCFC-124a Binding on NaX. 

J. Phys. Chem. B. 105, 12330-12337 (2001). 

M Ciraolo, J Hanson, C Grey. Solid-state rubidium 

exchange of zeolite NH4Y. Microporous Mesoporous 

Mater.. 49, 111-124 (2001). 

M Ciraolo, P Norby, J Hanson, D Corbin, C Grey. 

Structural characterization and 

Hydrochlorofluorocarbon Reactivity on Zin-Exchanged 

NaX. J. Phys. Chem. B. 103, 346-356 (1999). 

G Gainsford, N Robinson, J Tallon. 

(NH4)2(NH3(CH2)6NH3)4[H2W12O42].8H2O: a 

novel ammonium 1,6-hexanediammonium 

dodecatungstate. Acta Cryst. E. 58 (10), m521-m523 

(2002). 

A Gualtieri. Synthesis of sodium zeolites from a natural 

halloysite. Phys. Chem. Miner.. 28, 719-728 (2001). 

A Gualtieri. Study of NH4+ in the zeolite phillipsite by 

combined synchrotron powder diffraction and IR 

spectroscopy. Acta Cryst. B. B56, 584-593 (2000). 

T Jensen, R Hazell, A Christensen, J Hanson. 

Hydrothermal Synthesis of Lithium Zinc Phosphates: 

Structural Investigation of Twinned alphaLi4Zn(PO4)2 and a High Temperature Polymorph 

beta-Li4(PO4)2. J. Solid State Chem.. 166, 341-351 

(2002). 

A Kremenovic, P Norby, R Dimitrijevic, V Dondur. Hightemperature Synchrotron Powder Diffraction 

Investigation of the thermal Expansion, Strain and 

microstructure for the co-elastic a to fl Hexacelsian 

Transition. Phase Transit. 68, 587-605 (1999). 

H Liu. Structural and Functional Characterization of 

Inorganic Materials by Solid State NMR and 

Diffraction Techniques. PhD Thesis. State Univerity of 

New York, Stony Brook. (2001). 

J Post, P Heaney, J Hanson. Neutron and temperatureresolved synchrotron X-ray powder diffraction study 

of akaganÈite. Eighteenth International Mineralogical 

Association Meeting, Vol 18, p. 88, sponsored by 

International Mineralogical Association . (2002). 

J Post, P Heaney, J Hanson. Real-time synchrotron Xray powder diffraction studies of the structure and 

dehydration of todorokite. American Geophysical 

Union Spring Meeting, Vol 83, p. M22A-13, sponsored 

by American Geophysical Union. (2002). 

J Post, P Heaney, J Hanson. Rietveld refinement of a 

triclinic structure for synthetic Na-birnessite using 

synchrotron powder diffraction data. Powder Diffr.. 

17, 218-221 (2002). 

B Reisner, Y Lee, J Hanson, G Jones, J Parise, D 

Corbin, B Toby, A Freitag, J Larese, V Kahlenberg. 

Understanding negative thermal expansion and "trap 

door" cation relocations in zeolite RHO. Chem. 

Commun.. 22, 2221-2222 (2000). 

J Rodriguez, J Hanson, A Frenkel, J Kim, M Perez. 

Experimental and Theoretical Studies on the Reaction 

of H2 with NiO: Role of O Vacancies and Mechanism 

for Oxide Reduction. J. Am. Chem. Soc.. 124 (2), 

346-354 (2002). 

A Sani, G Cruciani, A Gualtieri. Dehydration dynamics 

of Ba-phillipsite: an in situ synchrotron powder 

diffraction study. Phys. Chem. Miner.. 29, 351-361 

(2002). 
7 - 9 Publications

K Taasti, A Christensen, P Norby, J Hanson, B Lebech, 

H Jakobsen, J Skibsted. Hydrothermal Synthesis, 

Single-Crystal Structure Analysis and Solid-State 

NMR Characterization of 

Zn2(oH)0.14(3)F0.86(3)(PO4). J. Solid State Chem.. 

164, 43-50 (2002). 

W Tong, G Xia, Z Tian, J Liu, J Cai, S Suib, J Hanson. 

Hydrothermal Synthesis and Characterization of 

Sodium Manganese Oxo-Phosphate Na2Mn2P(PO4)2 

H2O. Chem. Mater.. 14 (2), 615-620 (2002). 

Beamline X8C

M Alekshun, S Levy, T Mealy, B Seaton, J Head. The 

crystal structure of MarR, a regulator of multiple 

antibiotic resistance, at 2.3A resolution.. Nat. Struct. 

Biol.. 8, 710-714 (2001). 

R Batra, R Khayat, L Tong. Molecular mechanism for 

dimerization to regulate the catalytic activity of 

human cytomegalovirus protease. Nat. Struct. Biol.. 

8, 810-817 (2001). 

D Buckler, Y Zhou, A Stock. Evidence of intradomain 

and interdomain flexibility in an OmpR/PhoB homolog 

from Thermotoga maritima. Structure. 10 (2), 153-

164 (2002). 

D Desveaux, J Allard, N Brisson, J Sygusch. A New 

Family of Plant Transcription Factors Displays a Novel 

ssDNA-binding Surface. Nat. Struct. Biol.. 9 (7), 512-

517 (2002). 

P Dunten, C Belunis, R Crowther, K Hollfelder, U 

Kammlott, W Levin, H Michel, G Ramsey, A Swain, et 

al.. Crystal structure of human cytosolic 

phosphoenolpyruvate carboxykinase reveals a new 

GTP-binding site. J. Mol. Biol.. 316, 257-264 (2002). 

S Faham, J Bowie. Bicelle Crystallization: A new 

method for crystallizing membrane proteins yields a 

monomeric bacteriorhodopsin structure. J. Mol. Biol.. 

316, 1-6 (2002). 

D Fong, A Berghuis. Substrate Promiscuity of an 

Aminoglycoside Anitbiotic Resistance Enzyme via 

Target Mimicry. EMBO J.. 21 (10), 2323-2331 

(2002). 

P Hart, S Deep, A Taylor, Z Shu, C Hinck, A Hinck. 

Crystal Structure of the Human TBR2 ectodomainTGF-B3 Complex. Nat. Struct. Biol.. 9 (3), 203-208 

(2002). 

J Head, N Swamy, R Ray. Crystal Structure of the 

Complex Between Actin and Human Vitamin DBinding Protein at 2.5 Å Resolution . Biochemistry. 

41, 9015-9020 (2002). 

H Jayaram, Z Taraporewala, J Patton, B Prasad. 

Rotavirus protein involved in genome replication and 

packaging exhibits a HIT-like fold. Nature. 417, 311-

315 (2002). 

C Kim, M Gingery, R Pilpa, J Bowie. The SAM Domain of 

Polyhomeotic Forms a Helical Polymer. Nat. Struct. 

Biol.. 9 (6), 453-457 (2002). 

B Kwak, Y Zhang, M Yun, R Heath, C Rock, S 

Jackowski, H Park. Structure and Mechanism of 

CTP:Phosphocholine Cytidylyltransferase (LicC) from 

Streptococcus pneumoniae. J. Biol. Chem.. 277, 

4343-4350 (2002). 

C Lemke, P L. Howell. the 1.6Å structure og E. coli 

argininosuccinate synthetase suggests a 

conformational change during catalysis. Structure. 9, 

1153-1164 (2001). 

D Lim, N Strynadka. Structural Basis for the betalactam Resistance of PBP2a from Methicillin-resistant 

Staphylococcus aureus. Nat. Struct. Biol.. 9 (11), 870 

(2002). 

A Maris, M Sawaya, M Kaczor-Grzeskowiak, M Jarvis, S 

Bearson, M Kopka, I Schroder, R Gunsalus, R 

Dickerson. Dimerization Allows DNA Target Site 

Recognition by the NarL Response Regulator. Nat. 

Struct. Biol.. 9 (10), 771-778 (2002). 

C Regni, P Tipton, L Beamer. Crystal Structure of 

PMM/PMG: An Enzyme in the Biosynthetic Pathway of 

P. aeruginosa Virulence Factors. Structure Fold. Des.. 

10, 269-279 (2002). 

L Sampaleanu, B Yu, P L. Howell. Mutational Ananlysis 

of duck delta2 crytsallin and te structure of an 

inactve mutant with bound substrate provide insight 

into the enzymatic mechanism of argininosuccinate 

lyase. J. Biol. Chem.. 277 (7), 4166-4175 (2002). 

J Sivaraman, V Sauve, R Larocque, E Stura, J Schrag, 

M Cygler, A Matte. Structure of the 16S rRNA 

Pseudouridine Synthase RsuA Bound to Uracil and 

UMP. Nat. Struct. Biol.. 9, 353-358 (2002). 

S Soelaiman, K Jakes, N Wu, C Li, M Shoham. Crystal 

Structure of Colicin E3: Implications for Cell Entry 

and Ribosome Inactivation. Mol. Cell. 8, 1053-1062 

(2001). 

M Sundaramoorthy, M Meiyappan, P Todd, B Hudson. 

Crystal Structure of NC1 Domains; Structural Basis 

for Type IV Collagen Assembly in Basement 

Membranes. J. Biol. Chem.. 277 (34), 31142-33153 

(2002). 

W Vetter, D Gallagher, M Dudley. Synchrotron Whitebeam X-ray Topography of Ribonuclease S Crystals. 

Acta Cryst. D. D58, 579-584 (2002). 

S Wang, C Mura, M Sawaya, D Cascio, D Eisenberg. 

Structure of a Nudix protein from Pyrobaculum 

aerophilum reveals a dimer with two intersubunit 

beta sheets. Acta Cryst. D. 58, 571-578 (2002). 

Z Yang, H Zhang, H Hung, C Kuo, L Tsai, H Yuan, W 

Chou, G Chang, L Tong. Structural studies of the 

pigeon cytosolic NADP-dependent malic enzyme. 

Protein Sci.. 11, 332-341 (2002). 

L Zhang, J Doudna. Structural insights into group II 

intron catalysis and branch-site selection. Science. 

295, 2084-8 (2002). 

Beamline X9A

W Barton, J Biggins, J Jiang, J Thorson, D Nikolov. 

Expanding Pyrimidine Diphosphosugar Libraries via 

Structure-based Nucleotidylyltransferase Engineering. 

Proc Natl Acad Sci USA. 99 (21), 13397-13402 

(2002). 

W Barton, J Lesniak, J Biggins, P Jeffrey, J Jiang, K 

Rajashankar, J Thorson, D Nikolov. Structure, 

Mechanism and Engineering of a 

Nucleotidylytransferase as a First Step Toward 

Glycorandomization. Nat. Struct. Biol.. 8, 545-551 

(2001). 
Activity Report 2002 7 - 10 

J Bonanno, C Edo, N Eswar, U Pieper, M Romanowski, 

V Ilyin, S Gerchman, H Kycia, W Studier, et al.. 

Structural Genomics of Enzymes Involved in 

Sterol/Isoprenoid Biosynthesis. Proc Natl Acad Sci 

USA. 98, 12896-12901 (2001). 

M Bubb, L Govindasamy, E Yarmola, S Vorobiev, S 

Almo, T Somasundaram, M Chapman, M AgbandjeMcKenna, R McKenna. Polylysine Induces an 

Antiparallel Actin Dimer that Nucleates Filament 

Assembly: Crystal Structure at 3.5-A Resolution. J. 

Biol. Chem.. 277, 20999-21006 (2002). 

S Burley, K Kamada. Transcription Factor Complexes. 

Curr. Opin. Struct. Biol.. 12, 225-230 (2002). 

E Campbell, O Muzzin, M Chlenov, J Sun, C Olson, O 

Weinman, M Trester-Zedlitz, S Darst. Structure of the 

Bacterial RNA Polymerase Promoter Specificity Sigma 

Subunit. Mol. Cell. 9, 527-539 (2002). 

M Chance, A Bresnick, S Burley, J Jiang, C Lima, A Sali, 

S Almo, J Bonanno, J Buglino, et al.. Structural 

Genomics: A Pipeline for Providing Structures for the 

Biologist. Protein Sci.. 11, 723-738 (2002). 

J Coyle, S Qamar, K Rajashankar, D Nikolov. Structure 

of GABARAP in Two Conformations: Implications for 

GABA(A) Receptor Localization and Tubulin Binding. 

Neuron. 33, 63-74 (2002). 

R Deo, C Groft, K Rajashankar, S Burley. Recognition 

of the Rotavirus mRNA 3' Consensus by an 

Asymmetric NSP3 Homodimer. Cell. 108, 71-81 

(2002). 

M Finnin, J Donigian, N Pavletich. Structure of the 

Histone Deacetylase SIRT2. Nat. Struct. Biol.. 

20018, 621-625 (2001). 

G Gainsford. Crystals Great And Small. Chem. In New 

Zealand. 66 (2), 29-32 (2002). 

J Himanen, D Nikolov. Purification, Crystallization and 

Preliminary Characterization of the EphB2-ephrinB2 

Complex. Acta Cryst. D. D58, 533-535 (2002). 

J Himanen, K Rajashankar, M Lackmann, C Cowan, M 

Henkemeyer, D Nikolov. Crystal Structure of an Eph 

Receptor-ephrin Complex. Nature. 414, 933-938 

(2001). 

J Keift, K Zhou, A Grech, R Jubin, J Doudna. Crystal 

Structure of an RNA Tertiary Domain Essential to HCV 

IRES-Mediated Translation Initiation. Nat. Struct. 

Biol.. 9, 370-374 (2002). 

C Kielkopf, S Burley. X-ray Structures of Threonine 

Aldolase Complexes: Structural Basis of Substrate 

Recognition. Biochemistry. 41, 11711-11720 (2002). 

D Klein, T Schmeing, P Moore, T Steitz. The Kink-Turn: 

A New RNA Secondary Structure Motif. EMBO J.. 20, 

4214-4221 (2001). 

D Ostrov, M Roden, W Shi, E Palmieri, G Christianson, 

L Mendoza, G Villaflor, D Tilley, N Shastri, et al.. How 

H13 Histocompatibility Peptides Differing by a Single 

Methyl Group and Lacking Conventional MHC Binding 

Anchor Motifs Determine Self-Nonself Discrimination. 

J. Immunol.. 1, 283-289 (2002). 

S Roderick, W Chan, D Agate, L Olsen, M Vetting, K 

Rajashankar, D Cohen. Structure of human 

phosphatidylcholine transfer protein in complex with 

its ligand. Nat. Struct. Biol.. 9, 507-511 (2002). 

A Roll-Mecak, B Shin, T Dever, S Burley. Engaging the 

Ribosome: Universal IFs of Translation. Trends 

Biochem. Sci.. 26, 705-709 (2001). 

M Romanowski, R Soccio, J Breslow, S Burley. Crystal 

Structure of the Mus Musculus Cholesterol-regulated 

START Protein 4 (StarD4) Containing a StAR-related 

Lipid Transfer Domain. Proc Natl Acad Sci USA. 99

(10), 6949-6954 (2002). 

M Romanowski, S Burley. Crystal Structure of the 

Escherichia Coli Shikimate Kinase I (AroK) that 

Confers Sensitivity to Mecillinam. Proteins: Struc. 

Func. Genet.. 47 ( 4), 558-562 (2002). 

M Romanowski, S Gibney, S Burley. Crystal Structure 

of the Escherichia coli SbmC Protein That Protects 

Cells From the DNA Replication Inhibitor Microcin 

B17. Proteins: Struc. Func. Genet.. 47, 403ñ407 

(2002). 

M Romanowski, J Bonanno, S Burley. Crystal Structure 

of the Escherichia coli Glucose-Inhibited Division 

ProteinB(GidB) Reveals a Methyltransferase Fold. 

Proteins: Struc. Func. Genet.. 47, 563ñ567 (2002). 

M Romanowski, J Bonanno, S Burley. Crystal Structure 

of the Streptococcus Pneumoniae 

Phosphomevalonate Kinase, a Member of the GHMP 

Kinase Superfamily. Proteins: Struc. Func. Genet.. 47

( 4), 568-571 (2002). 

J Schwartz, X Zhang, S Nathenson, S Almo. Structural 

Mechanisms of Co-Stimulation. Nat. Immunol.. 5, 

427-434 (2002). 

W Shi, K Tanaka, T Crother, M Taylor, S Almo, V 

Schramm. Structural Analysis of Adenine 

Phosphoribosyltransferase from Saccharomyces 

Cerevisiae. Biochemistry. 36, 10800-10809 (2001). 

E Stavridi, Y Huyen, I Loreto, D Scolnick, T 

Halazonetis, N Pavletich, P Jeffrey. Crystal Structure 

of the FHA Domain of the Chfr Mitotic Checkpoint 

Protein and Its Complex with Tungstate.. Structure. 

10 (7), 891-9 (2002). 

Y Tseng, E Fedorov, J McCaffery, S Almo, D Wirtz. 

Micromechanics and Ultrastructure of Actin Filament 

Networks Crosslinked by Human Fascin: A 

Comparison with Alpha-Actinin. J. Mol. Biol.. 2, 351-

366 (2001). 

L Wang, C Lima, S Shuman. Structure and Mechanism 

of T4 Polynucleotide Kinase: an RNA Repair Enzyme. 

EMBO J.. 21 (14), 3873-3880 (2002). 

H Yang, P Jeffrey, J Miller, E Kinnucan, Y Sun, N 

Thoma, N Zheng, P Chen, N Zheng, et al. BRCA2 

Function in DNA Binding and Recombination from a 

BRCA2-DSS1-ssDNA Structure. Science. 297, 1837-

1848 (2002). 

X Zhang, J Schwartz, S Nathenson, S Almo. 

Crystallization and Preliminary X-Ray Analysis of the 

Complex Between Human CTLA-4 and B7-2. Acta 

Cryst. D. 57, 898-899 (2001). 

Beamline X9B

K Aghaiypour, A Wlodawer, J Lubkowski. Structural 

Basis for the Activity and Substrate Specificity of 

Erwinia Chrystanthemi L-Asparaginase . 

Biochemistry. 40, 5655-5664 (2001). 

B Ahvazi, H Kim, S Kee, Z Nemes, P Steinert. Threedimensional Structure of the Human 

Transglutaminase 3 Enzyme: Binding of Calcium Ions 

Changes Structure for Activation. EMBO J.. 21, 2055-

2067 (2002). 
7 - 11 Publications

B Ahvazi, H Kim, S Kee, Z Nemes, P Steinert. Related 

Articles Three-Dimensional Structure of the Human 

Transglutaminase 3 Enzyme: Binding of Calcium Ions 

Changes Structure for Activation . EMBO J.. 21, 

2055-2067 (2002). 

F Al-Mjeni, T Ju, T Pochapsky, M Maroney. XAS 

Investigation of the Structure and Function of Ni in 

Acireductone Dioxygenase. Biochemistry. 41, 6761-

6769 (2002). 

S Banumathi, K Rajashankar, C Notzel, B Aleksiev, T 

Singh, N Genov, C Betzel. Structure of the Neurotoxic 

Complex Vipoxin at 1.4 Å Resolution. Acta Cryst. D. 

57, 1552-1559 (2001). 

L Barrientos, J Louis, I Botos, T Mori, Z Han, B O'Keefe, 

M Boyd, A Wlodawer, A Gronenborn. The DomainSwapped Dimer of Cyanovirin-N is in a Metastable 

Folded State. Reconciliation of X-Ray and NMR 

Structures . Structure. 10, 673-686 (2002). 

J Blaszczyk, J Tropea, M Bubunenko, K Routzahn, D 

Waugh, D Court, X Ji. Crystallographic and Modeling 

Studies of RNase III Suggest a Mechanism for 

Double-Stranded RNA Cleavage. Structure. 9, 1225-

1236 (2001). 

J Blaszczyk, Y Li, H Yan, X Ji. Crystal Structure of 

Unligated Guanylate Kinase from Yeast Reveals GMPInduced Conformational Changes. J. Mol. Biol.. 307, 

247-257 (2001). 

I Botos, Z Wu, W Lu, A Wlodawer. Crystal Structure of 

a Cyclic Form of Bovine Pancreatic Trypsin Inhibitor. 

FEBS Lett. 509, 90-94 (2001). 

I Botos, B O'Keefe, S Shenoy, L Cartner, D Ratner, P 

Seeberger, M Boyd, A Wlodawer. Structures of the 

Complexeds of a Potent Anti-HIV Protein CyanovirinN and High Mannose Oligosaccharides. J. Biol. Chem.. 

277 (37), 34336-34342 (2002). 

J Boyington, P Sun. A Structural Perspective on MHC 

Class I Recognition by Killer Cell ImmunoglobulinLike Receptors . Mol. Immunol.. 38, 1007-1021 

(2002). 

J Boyington, A Brooks, P Sun. Structure of Killer Cell 

Immunoglobulin-Like Receptors and their Recognition 

of the Class I MHC Molecules. Immunol Rev.. 181, 

66-78 (2001). 

M Bucher, A Evdokimov, D Waugh. Differential Effects 

of Short Affinity Tags on the Crystallization of 

Pyrococcus Furiosus Maltodextrin-Binding Protein . 

Acta Cryst. D. 58, 392-397 (2002). 

C Chang, D Newton, S Rybak, A Wlodawer. 

Crystallographic and Functional Studies of a Modified 

Form of Eosinophil-Derived Neurotoxin (EDN) with 

Novel Biological Activities. J. Mol. Biol.. 317, 119-130 

(2002). 

R Chu, J Takei, J Knowlton, M Andrykovitch, W Pei, A 

Kajava, P Steinbach, X Ji, Y Bai. Redesign of a Fourhelix Bundle Protein by Phage Display Coupled with 

Proteolysis and Structural Characterization by NMR 

and X-ray Crystallography. J. Mol. Biol.. 323 (2), 

253-262 (2002). 

M Costas, J Rohde, A Stubna, Y Raymond, N Ho, L 

Quaroni, E Munck, L Que. A Synthetic Model for the 

Putatibe Fe IV 2O2 Diamond Core of Methane 

Monooxygenase Intermediate Q. J. Am. Chem. Soc.. 

123, 12931-12932 (2001). 

Z Dauter, D Adamiak. Anomalous Signal of Phosphorus 

used for Phasing DNA Oligomer: Importance of Data 

Redundancy. Acta Cryst. D. 57, 990-995 (2001). 

Z Dauter, M Dauter, E Dodson. Jolly SAD. Acta Cryst. 

D. D58, 494-506 (2002). 

U Derewenda, J Li, Z Derewenda, Z Dauter, G Mueller, 

G Rule, D Benjamin. The Crystal Structure of a Major 

Dust Mite Allergen Der p 2 and its Biological 

Implications. J. Mol. Biol.. 318, 189-197 (2002). 

M DiDonato, J Zhang, L Que, Jr., B Sarkar. Zinc 

Binding to the N-Terminal Domain of the Wilson 

Disease Copper-Transporting ATPase: Implications 

for in vivo Metal Ion Mediated Regulation of ATPase 

Activity. J. Biol. Chem.. 277, 13409 (2002). 

B Dunn, M Goodenow, A Gustchina, A Wlodawer. 

Retroviral Proteases. Genome Bio.. 3, 3006 (2002). 

A Evdokimov, D Anderson, K Routzahn, D Waugh. 

Unusual Molecular Architecture of the Yersinia Pestis 

Cytotoxin YopM: A Leucine-Rich Repeat Protein with 

the Shortest Repeating Unit. J. Mol. Biol.. 312, 807-

821 (2001). 

A Evdokimov, J Tropea, K Routzahn, D Waugh. ThreeDimensional Structure of the Type III Secretion 

Chaperone SycE from Yersinia Pestis. Acta Cryst. D. 

58, 398-406 (2002). 

M Frank, F Dyda, A Dobrodumov, A Gronenborn. Core 

Mutations Switch Monomeric Protein GB1 into an 

Intertwined Tetramer. Nat. Struct. Biol.. 9 (11), 877 

(2002). 

G Gainsford. Crystals Great And Small. Chem. In New 

Zealand. 66 (2), 29-32 (2002). 

X Gao, X Wen, C Yu, L Esser, S Tsao, B Quinn, L 

Zhang, L Yu, D Xia. The Crystal Structure of 

Mitochondrial Cytochrome bc1 in Complex with 

Famoxadone: The Role of Aromatic-Aromatic 

Interaction in Inhibition. Biochemistry. 41, 11692-

11702 (2002). 

S Garman, L Hannick, A Zhu, D Garboczi. The 1.9 

Angstrom Structure of alpha-NAcetylgalactosaminidase: Molecular Basis of 

Glycosidase Deficiency Diseases. Structure. 10, 425-

434 (2002). 

Y Gu, L Reshetnikova, Y Li, S Singh, X Ji. Crystal 

Structure of Shikimate Kinase from Mycobacterium 

tuberculosis Reveals the Dynamic Role of LID Domain 

in Catalysis. J. Mol. Biol.. 319, 779-789 (2002). 

J Gu, S Xu, L Yu. A Model of Cross-Bridge Attachment 

to Actin in the A.M.ATP State Based on X-Ray 

diffraction from Permeabilized Rabbit Psoas muscle. 

Biophys. J.. 82, 2123-2133 (2002). 

A Guarne, Q Zhao, R Ghirlando, W Yang. Insights into 

Negative Modulation of E. Coli Replication Initiation 

from the Structure of SeqA-hemimethylated DNA 

Complex. Nat. Struct. Biol.. 9 (11), 839 (2002). 

K Gunter, L Miller, M Aschner, R Eliseev, D Depuis, C 

Gavin, T Gunter. XANES Spectroscopy: A Promising 

Tool for Toxicology: A Tutorial. Neurotoxicology. 23, 

127 - 146 (2002). 

T Hall. Poly(A) Tail Synthesis and Regulation: Recent 

Structural Insights. Curr. Opin. Struct. Biol.. 1, 82-88 

(2002). 

A Henn, J Halfon, I Kela, I Orion, I Sagi. Nucleic Acid 

Fragmantation in Milliseconds Time scale Using a 

Convantional X-ray Rotating Anode Source. Nucleic 

Acids Res.. 29 (24), e122: 1-10 (2001). 
Activity Report 2002 7 - 12 

A Hofmann, M Grella, I Botos, W Filipowicz, A 

Wlodawer. Crystal Structures of the Semi-Reduced 

and Inhibitor-Bound Forms of Cyclic Nucleotide 

Phosphodiesterase from Arabidopsis Thaliana. J. Biol. 

Chem.. 277, 1419-1425 (2002). 

D Hoover, C Boulegue, D Yang, J Oppenheim, K 

Tucker, W Lu, J Lubkowski. The Structure of Human 

Macrophage Inflammatory Protein-3 alpha/CCL20 

Linking Antimicrobial and CC Chemokine Receptor-6-

Binding Activities with Human beta-Defensins. J. Biol. 

Chem.. 277 (40), 37647-37654 (2002). 

J Hurley, T Meyer. Subcellular Targeting by Membrane 

Lipids. Curr. Opin. Cell Biol.. 13, 146-152 (2001). 

J Hurley, D Anderson, B Beach, B Canagarajah, Y Ho, E 

Jones, G Miller, S Misra, M Pearson, et al. . Structural 

Genomics and Signaling Domains. Trends Biochem. 

Sci.. 27, 48-53 (2002). 

M Jaskolski, M Kozak, J Lubkowski, G Palm, A 

Wlodawer. Structures of Two Highly Homologous 

Bacterial L-Asparaginases: A Case of Enantiomorphic 

Space Groups. Acta Cryst. D. 57, 369-377 (2001). 

X Ji, J Blaszczyk, X Chen. The Absorption Edge of 

Protein-Bound Mercury and a Double-Edge Strategy 

for HgMAD Data Acquisition. Acta Cryst. D. D57, 

1003-1007 (2001). 

B Kang, D Cooper, Y Devedjiev, U Derewenda, Z 

Derewenda. The Structure of the FERM Domain of 

Merlin, the Neurofibromatosis Type 2 Gene Product. 

Acta Cryst. D. D58 (3), 381-391 (2002). 

S Kim, T Jeitner, P Steinert. Transglutaminases in 

Disease. Neurochem. Int.. 40, 85-103 (2002). 

H Kim, Z Nemes, W Idler, C Hyde, P Steinert, B Ahvazi. 

Crystallization and Preliminary X-Ray Analysis of 

Human Transglutaminase 3 from Zymogen to Active 

Form . J. Struct. Biol.. 135, 73-77 (2001). 

S Misra, G Miller, J Hurley. Recognizing 

Phosphatidylinositol 3-Phosphate. Cell. 107, 559-562 

(2001). 

S Misra, R Puertollano, Y Kato, J Bonifacino, J Hurley. 

Structural Basis for Acidic Cluster-Dileucine Signal 

Recognition by VHS Domains. Nature. 415, 933-937 

(2002). 

R Nagem, Z Dauter, I Polikarpov. Protein Crystal 

Structure Solution by Fast Incorporation of 

Negatively and Positively Charged Anomalous 

Scatterers. Acta Cryst. D. 57, 996-1002 (2001). 

V Oganesyan, N Oganesyan, S Terzyan, D Qu, Z 

Dauter, N Esmon, C Esmon. The Crystal Structure of 

the Endothelial Protein C Receptor and a Bound 

Phospholipid. J. Biol. Chem.. 277 (28), 24851-24854 

(2002). 

I Orion, F Dilmanian, Z Zhong, A Rosenfeld, I Sagi, A 

Henn , L PeÒa. X-Ray Synchrotron Beams for Medical 

Applications: Monte Carlo Simulations and 

Experiments Results. MC2000 ñ Monte Carlo 

Conference, 23-26 October 2000, Lisbon, Portugal, 

Vol 1, p. 93-98, sponsored by L. Tavora. (2000). 

A Padyana, V Bhat, K Madyastha, K Rajashankar, S 

Ramakumar. Crystal Structure of a Light-Harvesting 

Protein C-Phycocyanin from Spirulina Platensis. 

Biochem. Biophys. Res. Commun.. 282, 893-898 

(2001). 

M Perbandt, V Chandra, K Rajashankar, K Idakieva, K 

Parvanova, W Rypniewski, S Stoeva, W Voelter, N 

Genov, C Betzel. Preliminary X-Ray Diffraction 

Studies of the External Functional Unit RtH2-e from 

the Rapana Thomasiana. Acta Cryst. D. 57, 1663-

1665 (2001). 

L Quaroni, B Brazeau, A Rocklin, V Popescu, J 

Lipscomb, L Que, Jr.. EXAFS studies of mononuclear 

and dinuclear non-heme iron enzymes. J. Inorg. 

Biochem.. 86, 387 (2001). 

S Radaev, S Motyka, W Fridman, C Sautes-Fridman, P 

Sun. The Structure of a Human Type III Fc-Gamma 

Receptor in Complex with Fc. J. Biol. Chem.. 276, 

16469-16477 (2001). 

S Radaev, B Rostro, A Brooks, M Colonna, P Sun. 

Conformational Plasticity Revealed by the Cocrystal 

Structure of NKG2D and its Class I MHC-Like Ligand 

ULBP3. Immunity. 15, 1039-1049 (2001). 

S Radaev, P Sun. Recognition of IgG by Fcgamma 

Receptor. The Role of Fc Glycosylation and the 

Binding of Peptide Inhibitors. J. Biol. Chem.. 276, 

16478-16483 (2001). 

B Ramakrishnan, P Qasba. Crystal Structure of Lactose 

Synthase Reveals a Large Conformational Change in 

its Catalytic Component, the Beta-1,4-

Galactosyltransferase-I. J. Mol. Biol.. 310, 205-218 

(2001). 

B Ramakrishnan, P Qasba. Structure-based Design of 

beta1,4-galactosyltransferase I (b4Gal-T1) with 

Equally Efficient N-acetylgalactosaminyltransferase 

Activity: Point mutation broadens b4Gal-T1 donoe 

specificity. J. Biol. Chem.. 277 (23), 20833-20833 

(2002). 

B Ramakrishnan, P Balaji, P Qasba. Crystal Structure of 

Beta1,4-galactosyltransferase Complex with UDp-Gal 

Reveals an Oligosaccharide Acceptor Binding Site. J. 

Mol. Biol.. 318, 491-502 (2002). 

B Ramakrishnan, P Shah, P Qasba. Alpha-Lactalbumin 

(LA) Stimulates Milk Beta-1,4-Galactosyl-transferase 

I (BetaGal-T1) to Transfer Glucose from UDP-Glucose 

to N-acetylglucosamine. J. Biol. Chem.. 276, 37665-

37671 (2001). 

B Ramakrishnan, E Boeggeman, P Qasba. Beta-1,4-

Galactosyltransferase and Lactose Synthase: 

Molecular Mechanical Devices. Biochem. Biophys. 

Res. Commun.. 291, 1113-1118 (2002). 

J Rohde, M Costas, M Lim, W Nam, L Que, Jr.. EXAFS 

Studies of Biomimetic Intermediates Related to 

Active Species in Nonheme and Heme Iron Enzymes. 

8th International Symposium Activation of Dioxygen 

and Homogeneous Catalytic Oxidation, Atlanta, GA, 

U.S.A, 2002, p. 74, (2002). 

M Romanowski, J Bonanno, S Burley. Crystal Structure 

of the Streptococcus Pneumoniae 

Phosphomevalonate Kinase, a Member of the GHMP 

Kinase Superfamily. Proteins: Struc. Func. Genet.. 47

( 4), 568-571 (2002). 

J Shearer, H Jackson, D Schweitzer, D Rittenberg, T 

Leavy, W Kaminsky, R Scarrow, J Kovacs. The First 

Example of a Nitrile Hydratase Model Complex that 

Reversibly Binds Nitriles. J. Am. Chem. Soc.. 124

(38), 11417-11428 (2002). 
7 - 13 Publications

W Shi, A Sarver, C Wang, K Tanaka, S Almo, V 

Schramm. Closed Site Complexes of Adenine 

Phosphoribosyltransferase from Giardia Lamblia 

Reveal a Mechanism of Ribosyl Migration. J. Biol. 

Chem.. 277 (42), 39981 (2002). 

W Shi, L Basso, D Santos, P Tyler, R Furneaux, J 

Blanchard, S Almo, V Schramm. Structures of Purine 

Nucleoside Phosphorylase from Mycobacterium 

Tuberculosis in Complexes with Immucillin-H and its 

Pieces. Biochemistry. 28, 8204-8215 (2001). 

P Sun. To Kill or Not to Kill. Mol. Immunol.. 38, 1005-

1006 (2002). 

Q Tang, P Carrington, Y Horng, M Maroney, S 

Ragsdale, D Bocian. X-ray Absorption and Resonance 

Raman Studies of Methyl-Coenzyme M Reductase 

Indicating that Ligand Exchange and Macrocycle 

Reduction Accompany Reductive Activation. J. Am. 

Chem. Soc.. 124, 13242-13256 (2002). 

Y Tsujishita, S Guo, L Stolz, J York, J Hurley. Specificity 

Determinants in Phosphoinositide Dephosphorylation: 

Crystal Structure of an Archetypal Inositol 

Polyphosphate 5-Phosphatase. Cell. 105, 379-389 

(2001). 

X Wang, J McLachlan, P Zamore, T Tanaka Hall. 

Modular Recognition of RNA by a Human PumilioHomology Domain. Cell. 110, 501-512 (2002). 

X Wang, T Tanaka-Hall. Structural Basis for 

Recognition of AU-Rich Element RNA by the HuD 

Protein. Nat. Struct. Biol.. 8, 141-145 (2001). 

J Wang, H Ling, W Yang, R Craigie. Structure of a twodomain Fragment of HIV-1 Integrase: Implications 

for Domain Organization in the Intact Protein. EMBO 

J.. 20, 7333-7343 (2001). 

A Wlodawer, M Li, Z Dauter, A Gustchina, K Uchida, H 

Oyama, B Dunn, K Oda. Carboxyl Proteinase from 

Pseudomonas Defines a Novel Family of SubtilisinLike Enzymes. Nat. Struct. Biol.. 8, 442-446 (2001). 

A Wlodawer. Rational Approach to AIDS Drug Design 

Through Structural Biology. Annu. Rev. Med.. 53, 

595-614 (2002). 

A Wlodawer, M Li, A Gustchina, Z Dauter, K Uchida, H 

Oyama, N Goldfarb, B Dunn, K Oda. Inhibitor 

Complexes of the Pseudomonas Serine-Carboxyl 

Proteinase. Biochemistry. 40, 15602-15611 (2001). 

B Xiao, G Shi, J Gao, J Blaszczyk, Q Liu, X Ji, H Yan. 

Unusual Conformational Changes in 6-

hydroxymethyl-7,8-dihydropterin Pyrophosphokinase 

as Revealed by X-Ray Crystallography and NMR. J. 

Biol. Chem.. 276, 40274-40281 (2001). 

S Xu, J Gu, G Melvin, L Yu. Structural Characterization 

of Weakly Attached Cross-Bridges in the A.M.ATP 

State in Permeabilized Rabbit psoas Muscle. Biophys. 

J.. 82, 2111-2122 (2002). 

S Xu, J Gu, T Rhodes, B Belknap, G Rosenbaum, G 

Offer, H White, L Yu. The M.ADP.Pi State is Required 

for helical Order in the Thick Filaments of Skeletal 

Muscle. Biophys. J.. 77, 2665-2676 (1999). 

Beamline X10A

J Barnes, W Bras. Tempature-Induced Contrast 

Variation as a Tool for Characterizing Anisotropic 

Polymer Microstructures. Advances in X-ray 

Analaysis, Denver X-ray Conference 2001, Vol 45, p. 

72-77, sponsored by ICDD. (2002). 

W Hu, S Srinivas, E Sirota. Crystalline Structure and 

Properties of EP and EB Copolymers by Solid-State 

NMR, DSC, and WAXS. Macromolecules. 35, 5013-

5024 (2002). 

S Idziak, S Welch, M Kisilak, C Mugford, G Potvin, L 

Veldhuis, E Sirota. Undulating membrane structure 

under mixed extensional-shear. Eur. Phys. J. D. 6, 

139-145 (2001). 

H Iwamato, K Oiwa, T Suzuki, T Fujisawa. States of 

Thin Filament Regulatory Proteins as Revealed by 

Combined Cross-linking/X-ray Diffraction Techniques. 

J. Mol. Biol.. 317 (5), 707-720 (2002). 

M Kisilak, H Anderson, N Babcock, M Stetzer, S Idziak, 

E Sirota. An x-ray extensional flow cell. Rev. Sci. 

Instrum.. 72 (11), 4305-4307 (2001). 

B Mishra, B Thomas. Phospholipid/Protein Cones. J. 

Am. Chem. Soc.. 124, 6866-6871 (2002). 

C Nuckolls, R Shao, W Jang, N Clark, D Walba, T Katz. 

Electro-Optic Switching by Helicene Liquid Crystals. 

Chem. Mater.. 14 (2), 773-776 (2002). 

B Thomas, C Lindemann, R Corcoran, C Cotant, J 

Kirsch, P Persichini. Phosphonate Lipid Tubules II. J. 

Am. Chem. Soc.. 124 (7), 1227-1233 (2002). 

T Thurn-Albrecht, J DeRouchey, T Russell, R Kolb. 

Pathways Toward Electric Field Induced Alignment of 

Block Copolymers. Macromolecules. 35, 8106-8110 

(2002). 

S Welch, M Stetzer, G Hu, E Sirota, S Idziak. 

Intermembrane spacing and velocity profiling of a 

lamellar lyotropic complex fluid under flow using xray diffraction. Phys. Rev. E. 65 (6), 061511/1-6 

(2002). 

Beamline X10B

S Welch, M Stetzer, G Hu, E Sirota, S Idziak. 

Intermembrane spacing and velocity profiling of a 

lamellar lyotropic complex fluid under flow using xray diffraction. Phys. Rev. E. 65 (6), 061511/1-6 

(2002). 

W Zhang, B Fu, Y Seo, E Schrag, B Hsiao, P Mather, N 

Yang, D Xu, H Ade, et al. Effect of Methyl 

Methacrylate/Polyhedral Oligomeric Silsequioxane 

Random Copolymers in Compatibilizatin of 

Polystyrene and Poly(methyl methacrylate) Blends. 

Macromolecules. 35, 8029-8038 (2002). 

Beamline X10C

M Jaime Vasquez, G Halada, C Clayton. The Application 

of Synchrotron-based Spectroscopic Techniques to 

the Study of Chromate Conversion Coatings. 

Electrochim. Acta. 47 (19), 3105-3115 (2002). 

M Jaime Vasquez, G Halada, C Calyton, J Longtin. On 

the Nature of the Chromate Conversion Coating 

Formed on Intermetallic Constituents of AA2024-T3. 

Surf. Interface Anal.. 33 (7), 607-616 (2001). 

M Vasquez, G Halada, C Clayton. Composition of 

Chromate Conversion Coatings Formed on 

multilayered Thin Films of AA2024-T3 matrix and 

Al2Cu, Al2CuMg and Al20Cu2(FeMn).. Vol PV2001-

22, p. 444-453, (2001). 
Activity Report 2002 7 - 14 

M Vasquez, G Halada, C Clayton, J Longtin. 

Composition of Surface Treated Thin Films Analogs of 

Intermetallic Constituents in AA2024-T3. Corrosion 

and Corrosion Prevention of Low Density Metal and 

Alloys, Vol PV2000-23, p. 57-68, sponsored by The 

Electrochemical Society. (2001). 

M Vasquez, G Halada, C Clayton, J Longtin. Effects of 

Aging on Chromate Conversion Coatings Formed on 

AA2024-T3 and Some Intermetallic Constituents. 

Corrosion and Corrosion Prevention of Low Density 

Metals and Alloys, Vol PV2000-23, p. 101-113, 

sponsored by Electrochemical Society. (2001). 

Beamline X11A

Y Arai, D Sparks. Residence Time Effects on Arsenate 

Surface Speciation at the Aluminum Oxide-water 

Interface. Soil Sci. 167, 303-314 (2002). 

A Argo, B Gates. Propene Hydrogenation Catalyzed by 

?-Al2O3 - Supported Ir4 Clusters: Inhibition by 

Dehydrogenated Propene Derivatives on Ir4. 

Langmuir. 18 (6), 2183-2189 (2002). 

A Argo, J Odzak, F Lai, B Gates. Observation of Ligand 

Effects during Alkene Hydrogenation Catalysed by 

Supported Metal Clusters. Nature. 415, 623-626 

(2002). 

S Calvin, E Carpenter, V Harris, S Morrison. Use of 

multiple-edge refinement of extended x-ray 

absorption fine structure to determine site occupancy 

in mixed ferrite nanoparticles. Appl. Phys. Lett.. 81

(20), 3828-3830 (2002). 

R D‰hn, A Scheidegger, A Manceau, M Schlegel, B 

Baeyens, M Bradbury, M Morales. Neoformation of Ni 

phyllosilicate upon Ni uptake on montmorillonite. A 

kinetics study by powder and polarized EXAFS. 

Geochim. Cosmochim. Acta. 66 (13), 2335-2347 

(2002). 

L Dieng, A Ignatov, T Tyson, M Croft, F Dogan, C Kim, 

J Woicik, J Grow. Observation of changes in the 

atomic and electronic structure of single-crystal 

YBa2Cu3O6.6 accompaying bromination. Phys. Rev. 

B: Condens. Matter. 66, 014508 (2002). 

C Dodge, A Francis. Photodegradation of a ternary 

iron(III)-uranium(VI)-citric acid complex. Environ. 

Sci. Tech.. 36, 2094-2100 (2002). 

C Dodge, A Francis, J Gillow, G Halada, C Eng, C 

Clayton. Association of uranium with iron oxides 

typically formed on corroding steel surfaces. Environ. 

Sci. Tech.. 36 (16), 3504-3511 (2002). 

E Elzinga, R Reeder, S Withers, R Peale, R Mason, K 

Beck, W Hess. EXAFS Study of Rare-earth Element 

Coordination in Calcite. Geochim. Cosmochim. Acta. 

66 (16), 2875-2885 (2002). 

E Elzinga, R Reeder. X-ray absorption spectroscopy 

study of Cu2+ and Zn2+ adsorption complexes at the 

calcite surface: Implications for site-specific metal 

incorporation preferences during calcite crystal 

growth. Geochim. Cosmochim. Acta. 66 (22), 3943-

3954 (2002). 

E Elzinga, D Sparks. X-ray Absorption Spectroscopy 

Study of the Effects of pH and Ionic Strength on 

Pb(II) Sorption to Amorphous Silica . Environ. Sci. 

Tech.. 36, 4352-4357 (2002). 

E Ghabbour, A Scheinost, G Davies. XAFS Studies of 

Cobalt(ll) Binding by Peat, Plant and Soil Derived 

Solid Humic Acids. The 20th Anniversary Conference 

of the International Humic Substances Society , Vol 

IHSS 11, p. 277-282, sponsored by International 

Humic Substances Society. (2002). 

E Ghabbour, A Scheinost, G Davies. XAFS Studies of 

Cobalt(ll) Binding by Peat, Plant and Soil Derived 

Solid Humic Acids. Synchrotron Environmental 

Science-II Conference, May 6-8, 2002 , Vol II, p. 40, 

sponsored by Advanced Photon Source. (2002). 

J Goellner, J Guzman, B Gates. Synthesis and Structure 

of Tetrairidium Clusters on TiO2 Powder: 

Characterization by Infrared and Extended X-ray 

Absorption Fine Structure Spectroscopies. J. Chem. 

Phys.. 106 (6), 1229-1238 (2002). 

S Heifets, G Stupakov, S Krinsky. CSR Instability in a 

Bunch Compressor. Phys. Rev. ST AB. 5, 064401 

(2002). 

Y Lee, R Reeder, R Wenskus, E Elzinga. Structural 

relaxation in the MnCO3-CaCO3 solid solution: a Mn 

K-edge EXAFS study. Phys. Chem. Miner.. 29, 585-

594 (2002). 

S Maeng, L Axe, T Tyson. Characterization of GunBarrel Steel Corrosion as a Function of Time in 

Concentrated Hydrochloric Acid Solution. 

Organometallics. 58 (4), 370-380 (2002). 

A Mansour, A Marcelli, G Cibin, G Yalovega, T 

Sevastyanova, A Soldatov. Amorphous 

Al_90Fe_xCe_10-x alloys: X-ray Absorption Analysis 

of the Al, Fe, and Ce Local Atomic and Electronic 

Structures. Phys. Rev. B. 65, 134207 (2002). 

A Mansour, P Smith, W Baker, M Balasubramanian, J 

McBreen. In situ XAS investigation of the oxidation 

state and local structure of vanadium in discharged 

and charged V2O5 aerogel cathodes. Electrochim. 

Acta. 47, 3151-3161 (2002). 

A Mansour, S Dallek, P Smith, W Baker. 

Thermogravimetry and X-Ray Absorption 

Spectroscopy Study of Heated V2O5.nH2O Aerogels 

and Ambigels. J. Electrochem. Soc.. 149 (12), 

A1589-A1597 (2002). 

D Peak, D Sparks. Mechanisms of Selenate Adsorption 

on Iron Oxides and Hydroxides. Environ. Sci. Tech.. 

36, 1460-1466 (2002). 

J Qian. Mercury species in environmental samples 

studied by spectroscopic methods. Ph.D. Thesis. 

Department of Forest Ecology, Swedish University of 

Agricultural Sciences, UmeÂ. (2001). 

B Ravel, V Harris, E Carpenter. Oxidation of iron in 

iron/gold core/shell nanoparticles. J. Appl. Phys.. 91

(10), 8195 (2002). 

B Ravel, M Raphael, V Harris, Q Huang. EXAFS and 

Neutron Diffraction Studies of the Heusler Alloy 

Co2MnSi. Phys. Rev. B. 65 (18), 184431 (2002). 

D Roberts, A Scheinost, D Sparks. Zinc Speciation in a 

Smelter-Contaminated Soil Profile Using Bulk and 

Microspectroscopic Techniques. Environ. Sci. Tech.. 

36, 1742-1750 (2002). 

K Scheckel, J Ryan. Effects of Aging and pH on 

Dissolution Kinetics and Stability of 

Chloropyromorphite. Environ. Sci. Tech.. 36 (10), 

2198-2204 (2002). 
7 - 15 Publications

P Trivedi, L Axe, T Tyson. An Analysis of Zinc Sorption 

to Amorphous versus Crystalline Iron Oxides using 

XAS. J. Colloid Interface Sci.. 244, 230-238 (2001). 

P Trivedi, L Axe, T Tyson. XAS Studies of Ni and Zn 

Sorbed to Hydrous Manganese Oxide. Environ. Sci. 

Tech.. 35, 4515-4521 (2001). 

Beamline X12B

A Avgeropoulos, S Paraskeva, N Hadjichristidis, E 

Thomas. Synthesis and Microphase Separation of 

Linear Triblock Terpolymers of Polystyrene, High 1,4-

Polybutadiene, and High 3,4-Polyisoprene. 

Macromolecules. 35, 4030-4035 (2002). 

M Baniecki, W McGrath, Z Dauter, W Mangel. 

Adenovirus proteinase: crystallization and preliminary 

X-ray diffraction studies to atomic resolution. Acta 

Cryst. D. D58, 1462-1464 (2002). 

B Gibbons, P Roach, T Hurley. Crystal Structure of the 

Autocatalytic INitiator of Glycogen Biosynthesis, 

Glycogenin. J. Mol. Biol.. 319 (2), 463-477 (2002). 

I Hayashi, K Vuori, R Liddington. The focal adhesion 

targeting (FAT) domain of focal adhesion kinase is a 

four-helix bundle that binds paxillin. Nat. Struct. 

Biol.. 9 (2), 101-109 (2002). 

M Lemieux, R Reithmeier, D Wang. Importance of 

detergent and phospholipid in the crystallization of 

the human erythrocyte anion-exchanger membrane 

domain.. J. Struct. Biol.. 137 (3), 322-32 (2002). 

B Mahalingam, P Boross, Y Wang, J Louis, C Fischer, J 

Tozser, R Harrison, I Weber. Combining mutations in 

HIV-1 protease to understand mechanisms of 

resistance. Proteins: Struc. Func. Genet.. 48, 107-

116 (2002). 

M McDonough, J Anderson, N Silvaggi, R Pratt, J Knox, 

J Kelly. Structures of Two Kinetic Intermediates 

Reveal Species Specificity of Penicillin-Binding 

Proteins. J. Mol. Biol.. 322 (1), 111-122 (2002). 

V Oganesyan, N Oganesyan, S Terzyan, D Qu, Z 

Dauter, N Esmon, C Esmon. The Crystal Structure of 

the Endothelial Protein C Receptor and a Bound 

Phospholipid. J. Biol. Chem.. 277 (28), 24851-24854 

(2002). 

J Petock, I Torshin, Y Wang, G DuBois, C Croce, R 

Harrison, I Weber. Structure of murine Tcl1 at 2.5A 

resolution and implications for the TCL oncogene 

family. Acta Cryst. D. D57, 1545-1551 (2001). 

P Smith, S Firestein, J Hunt. Crystal Structure of 

Olfactory Marker Protein at 2.3 A resolution. J. Mol. 

Biol.. 319 (3), 807-821 (2002). 

Beamline X12C

P Arjunan, N Nemeria, A Brunskill, K Chandrasekhar, M 

Sax, Y Yan, F Jordan, J Guest, W Furey. Structure of 

the Pyruvate Dehydrogenase Multienzyme Complex 

E1 Component from Escerichia coli at 1.85 Angstrom 

Resolution. Biochemistry. 41 (16), 5213-5221 

(2002). 

P Bar On, C Millard, M Harel, H Dvir, A Enz, J Sussman, 

I Silman. Kinetic ane Structural Studies on the 

Interaction of Cholinesterases with the AntiAlzheimer Drug Rivastigmine. Biochemistry. 41 (11), 

3555-3564 (2002). 

S Benson, J Bamford, D Bamford, R Burnett. The X-ray 

crystal structure of P3, the major coat protein of the 

lipid-containing bacteriophage PRD1, at 1.65 Å 

resolution. Acta Cryst. D. 58, 39-59 (2002). 

M Bewley, C Marohnic, M Barber. The structure and 

biohcemistry of NADH-dependent cytochrome b5 

reductase are now consistent. Biochemistry. 40 (45), 

13574-13582 (2001). 

J Brown, K Kim, G Jun, N Greenfield, R Dominguez, N 

Volkmann, S Hitchcock-DeGregori, C Cohen. 

Deciphering the design of the tropomyosin molecule.. 

Proc Natl Acad Sci USA. 98 (15), 8496-8501 (2001). 

B Brown, A Athanasiadis, E Hanlon, K Lowenhaupt, C 

Wilbert, A Rich. Crystallization of the Za Domain of 

the Human Editing Enzyme ADAR1 Complexed with a 

DNA-RNA Chimeric Oligonucleotide in the Lefthanded Z-conformation. Acta Cryst. D. 58 (1), 120-

123 (2002). 

C Ceccarelli, N Grodsky, N Ariyaratne, R Colman, B 

Bahnson. Crystal Structure of Porcine Mitochondrial 

NADP+-dependent Isocitrate Dehydrogenase 

Complexed with Mn2+ and Isocitrate. J. Biol. Chem.. 

277 (45), 43454-43462 (2002). 

X Chen, S Schauder, N Potier, A Van Dorsselaer, I 

Pelczer, B Bassler, F Hughson. Structural 

Identification of a Bacterial Quorum-Sensing Signal 

Containing Boron. Nature. 415 (6871), 545-549 

(2002). 

C Chen, H Zhang, A Kim, A Howard, G Sheldrick, D 

Mariano-Dunaway, O Herzberg. Degradition Pathway 

of the Phosphonate Ciliatine: Crystal Structure of 2-

Aminoethylphosphonate Transaminase. Biochemistry. 

41, 13162-13169 (2002). 

S Dhe-Paganon, K Duda, M Iwamoto, Y Chi, S 

Shoelson. Crystal Structure of the HNF4 alpha Ligand 

Domain in Complex with Endogenous Fatty Acid 

Ligand. J. Biol. Chem.. 277, 37973-37976 (2002). 

H Dvir, D Wong, M Harel, X Barril, M Orozco, F Luque, 

P Camps, T Rosenberry, I Silman, J Sussman. 3D 

Structure of Torpedo californica Acetylcholinesterase 

Complexed with Huprine X at 2.1 A Resolution: 

Kinetic and Molecular Dynamic Correlates. 

Biogeochemistry. 41 (9), 2970-2981 (2002). 

S Eswaramoorthy, D Kumaran, S Swaminathan. A 

Novel Mechanism for Clostridium Botulinum 

Neurotoxin Inhibition. Biochemistry. 41, 9795-9802 

(2002). 

H Feinberg, D Mitchell, K Drickamer, W Weis. 

Structural Basis for Selective Recognition of 

Oligosaccharides by DC-SIGN and DC-SIGNR. 

Science. 294, 2163-2166 (2001). 

A Ferguson, R Chakraborty, B Smith, L Esser, D van 

der Helm, J Deisenhofer. Structural basis of gating by 

the outer membrane transporter FecA. Science. 295, 

1715-1719 (2002). 

B Gibbons, P Roach, T Hurley. Crystal Structure of the 

Autocatalytic INitiator of Glycogen Biosynthesis, 

Glycogenin. J. Mol. Biol.. 319 (2), 463-477 (2002). 

O Herzberg, C Chen, S Liu, A Tempczyk, A Howard, M 

Wei, D Ye, D Dunaway-Mariano. Pyruvate Site of 

Pyruvate Phosphate Dikinase: Crystal Structure of 

the Enzyme-Phosphonopyruvate Complex, and 

Mutant Analysis. Biochemistry. 41 (3), 780-787 

(2002). 
Activity Report 2002 7 - 16 

Q Huai, H Kim, Y Liu, Y Zhao, A Mondragon, J Liu, H 

Ke. Crystal Structure of Calcineurin-cyclophilincyclosporin shows Common but Distinct Recognition 

of Immunophilin-drug Complexs. Proc Natl Acad Sci 

USA. 99 (19), 12037-12042 (2002). 

J Hunt, S Weinkauf, L Henry, J Fak, P McNicholas, D 

Oliver, J Deisenhofer. Nucleotide Control of 

Interdomain Interactions in the Conformational 

Reaction Cycle of SecA. Science. 297, 2018-2026 

(2002). 

K Jude, S Wright, C Tu, D Silverman, R Viola, D 

Christianson. Crystal Structure of F65A/Y131CMethylimidazole Carbonic Anhydrase V Reveals 

Architectural Features of an Engineered Proton 

Shuttle. Biochemistry. 41 (8), 2485-2491 (2002). 

T Keating, C Marshall, C Walsh, A Keating. The 

Structure of VibH Represents Nonribosomal Peptide 

Synthetase Condensatoin, Cyclization and 

Epimerization Domains. Nat. Struct. Biol.. 9 (7), 522-

526 (2002). 

W Li, S Srinivasula, J Chai, P Li, J Wu, Z Zhang, E 

Alnemri, Y Shi. Structural Insights into the ProApoptotic Function of Mitochondrial Serine Protease 

HtrA2/Omi. Nat. Struct. Biol.. 9 (6), 436-441 (2002). 

K Lim, H Zhang, A Tempczyk, N Bonander, J Toedt, A 

Howard, E Eisenstein, O Herzberg. Crystal structure 

of YecO from Haemophilus influenzae (HI0319) 

reveals a methyltransferase fold and a bound Sadenosylhomocysteine. Proteins: Struc. Func. Genet.. 

45, 397-407 (2001). 

Y Luo, M Bertero, E Frey, R Pfuetzner, M Wenk, L 

Creagh, S Marcus, D Lim, F Sicheri, et al. Structural 

and Biochemical Characterization of the Type III 

Secretion Chaperones CesT and SigE. Nat. Struct. 

Biol.. 8, 1031-1036 (2001). 

J Madrazo, J Brown, S Litvinovich, R Dominguez, S 

Yakovlev, L Medved, C Cohen. Crystal structure of 

the central region of bovine fibrinogen (E5 fragment) 

at 1.4 Å resolution.. Proc Natl Acad Sci USA. 98 (21), 

11967-11972 (2001). 

M McDonough, J Anderson, N Silvaggi, R Pratt, J Knox, 

J Kelly. Structures of Two Kinetic Intermediates 

Reveal Species Specificity of Penicillin-Binding 

Proteins. J. Mol. Biol.. 322 (1), 111-122 (2002). 

J Min, X Zhang, X Cheng, S Grewal, R Xu. Structure of 

the SET Domain Histone Lysine Methyltransferase 

Clr4. Nat. Struct. Biol.. 9 (11), 828 (2002). 

K Newberry, Y Hou, J Perona. Structural Origins of 

Amino Acid Selection without Editing by CysteinyltRNA Synthetase. EMBO J.. 21 (11), 2778-2787 

(2002). 

J Parsons, K Lim, A Tempczyk, E Eisenstein, O 

Herzberg. From Structure to Function: YrbI from 

Haemophilus influenzae (HI1679) is a Phosphatase. 

Proteins: Struc. Func. Genet.. 46, 394-404 (2002). 

D Shi, R Gallegos, J DePonte III, H Morizono, X Yu, N 

Allewell, M Malamy, M Tuchman. Crystal structure of 

a transcarbamylase-like protein from the anaerobic 

bacterium Bacteroides fragilis at 2.0 A resolution.. J. 

Mol. Biol.. 320, 899 (2002). 

J Sivaraman, V Sauve, R Larocque, E Stura, J Schrag, 

M Cygler, A Matte. Structure of the 16S rRNA 

Pseudouridine Synthase RsuA Bound to Uracil and 

UMP. Nat. Struct. Biol.. 9, 353-358 (2002). 

P Smith, S Firestein, J Hunt. Crystal Structure of 

Olfactory Marker Protein at 2.3 A resolution. J. Mol. 

Biol.. 319 (3), 807-821 (2002). 

E Sundberg, M Sawicki, S Southwood, P Andersen, A 

Sette, R Mariuzza. Minor Structural Changes in 

Mutated Human Melanoma Antigen Correspond to 

Dramatically Enhanced Stimulation of a CD4+ Tumorinfiltrating Lymphocyte Line. J. Mol. Biol.. 319 (2), 

449-461 (2002). 

J Till, M Becerra, A Watty, Y Lu, Y Ma, T Neubert, S 

Burden, S Hubbard. Crystal structure of the MuSK 

tyrosine kinase: insights into receptor autoregulation. 

Structure. 10, 1187-1196 (2002). 

P Van Roey, L Meehan, J Kowalski, M Belfort, V 

Derbyshire. Catalytric domain structure and 

hypothesis for function of GIY-YIG intron 

endonuclease I-TevI. Nat. Struct. Biol.. 9 (11), 806-

811 (2002). 

T Wan, R Beavil, S Fabiane, A Beavil, M Sohi, M 

KEown, R Young, A Henry, R Owens, et al.. The 

crystal structure of IgE Fc reveals an asymmetrically 

bent conformation. Nat. Immunol.. 3 (7), 681-686 

(2002). 

Z Yang, G Spraggon, L Pandi, S Everse, M Riley, R 

Doolittle. Crystal structure of fragment D from 

lamprey fibrinogen complexed with the peptide GlyHis-Arg-Pro-amide. Biochemistry. 41 (32), 10218-

10224 (2002). 

Z Zhang, M Hayashi, O Merkel, B Stillman, R Xu. 

Structure and Function of the BAH-containing Domain 

of Orc1p in Epigenetic Silencing. EMBO J.. 21 (17), 

4600-4611 (2002). 

Beamline X13B

J Ablett, C Kao, A Lunt. The Design and Performance Of 

An X-Ray Micro-Focusing System Using Differentially 

Deposited Elliptical Mirrors At The National 

Synchrotron Light Source. Rev. Sci. Instrum.. 73

(10), 3464-3468 (2002). 

L Berman, P Siddons, P Montanez, A Lenhard, Z Yin. A 

Cryogenically Cooled Channel-cut Crystal 

Monochromator Using a Helium Refrigerstor and Heat 

Exchanger. Rev. Sci. Instrum.. 73 (3), 1481-1484 

(2002). 

Y Hasegawa, Y Ueji, K Okitsu, J Ablett, D Siddons, Y 

Amemiya. Transmission-type X-ray linear polarizer 

with perfect crystals. J. Synch. Rad.. 5 (3), 738-740 

(1998). 

Beamline X14A

J Bai, C Sparks, G Ice. Monte Carlo Ray-Tracing Error 

Analysis of a Sagittal-Focusing Optical System as 

Applied to Synchrotron Radiation. Rev. Sci. Instrum.. 

73 (3), 1499-1501 (2002). 

J Kim. Effect of the Substrate-Induced Crystalline 

Interphase on the Adhesion of Polyurethane to 

Metals. Ph. D. Thesis. The Pennsylvania State 

University, (2001). 

J Li. X-ray characterization of CuPt-ordered 

semiconductor alloy films. Spontaneous Ordering in 

Semiconductor Alloys, Plenum Press/ Kluwer 

Academic, (2002). 
7 - 17 Publications

J Li, R Forrest, S Moss, Y Zhang, A MAscarenhas, J Bai. 

Determination of the order parameter of CuPt-B 

ordered GaInP2 films by x-ray diffraction. J. Appl. 

Phys.. 91 (11), 9039-9042 (2002). 

Q Qian, T Tyson, C Dubourdien, A Bossak, J Se'nateur, 

M Deleon, J Bai, G Bonfait. Structural studies of 

annealed ultrathin La0.8 MnO3 films. Appl. Phys. 

Lett.. 80 (15), 2663-2665 (2002). 

C Rawn, C Jones, B Chakoumakous, S Marchall, L 

Stern, S Kirby, Y Ishii, B Toby. (2001). 

J Rho, S Mishra, K Chung, J Bai, G Pharr. The 

relationship between microstructure and the 

nanoindentation properties of intramuscular herring 

bone. Ann. Biomed. Eng.. 29 (12), 1082-1088 

(2001). 

T Watkins, A McMillan, R Lauf, A Eberhardt. (2001). 

P Williams, J Biernacki, L Walker, H Meyer, C Rawn, J 

Bai. Microanalysis of alkali-activated fly ash-CH 

pastes. Cem. Concr. Res.. 32 (6), 963-972 (2002). 

H Woo. Structural, Transport and Magnetic Studies of 

Perovskite Bi1-xCaxMnO3. Ph. D. Thesis. New Jersey 

Institute of Technology, New Jersey. (2001). 

Beamline X15A

M Kiss, D Sayers, Z Zhong. Comparison of X-ray 

detectors for a diffraction enhanced imaging system. 

Nucl. Instrum. Meth. A. 491, 280-290 (2002). 

I Orion, F Dilmanian, Z Zhong, A Rosenfeld, I Sagi, A 

Henn , L PeÒa. X-Ray Synchrotron Beams for Medical 

Applications: Monte Carlo Simulations and 

Experiments Results. MC2000 ñ Monte Carlo 

Conference, 23-26 October 2000, Lisbon, Portugal, 

Vol 1, p. 93-98, sponsored by L. Tavora. (2000). 

B Tinkham. X-ray Investigation of the initial growth of 

Si/Ge/Si Heterostructures grown by Surfactant 

Mediated Epitaxy. Ph.D. Thesis. Northwestern 

University, Evanston. (2002). 

S Warren, A Reitzle, A Kazimirov, J Ziegler, O Bunk, L 

Cao, F Renner, D Kolb, M Bedzyk, J Zegenhagen. A 

structure study of electrodeposited Au on Si(111). 

Surf. Sci.. 496, 287 - 298 (2002). 

J Ziegler, O Bunk, G Scherb, A Kazimirov, L Cao, D 

Kolb, R Johnson, J Zegenhagen. Pb deposition on nSi(111):H electrodes: an in-situ x-ray study. Surf. 

Sci.. 452, 150 - 160 (2000). 

J Ziegler, A Reitzle, O Bunk, J Zegenhagen, D Kolb. 

Metal deposition on n-Si(111):H electrodes. 

Electrochim. Acta. 45, 4599 - 4605 (2000). 

Beamline X15B

P Citrin, D Hamann, P Northrup. Erbium in Si and GaN: 

extended versus point defects. Physica B. 308 (1), 

369 (2001). 

P Voyles, D Muller, J Grazul, P Citrin, H Gossmann. 

Atomic-scale imaging of individual dopant atoms and 

clusters in highly n-type bulk Si. Nature. 416 (6883), 

826 - 829 (2002). 

Beamline X16A

R Drautz, H Reichert, M F‰hnle, H Dosch, J Sanchez. 

Spontaneous L12 Order at Ni90Al10(110) Surfaces: 

An X-ray and First-Principles-Calculation Study. Phys. 

Rev. Lett.. 87 (23), 236102 (2001). 

I Robinson, P Bennett, F Himpsel. Structure of 

Quantum Wires in Au/Si(557). Phys. Rev. Lett.. 88, 

096104-1 (2002). 

Beamline X16B

Y Soh, P Evans, Z Cai, B Lai, C Kim, G Aeppli, N 

Mathur, M Blamire, E Isaac. Local Mapping of Strain 

at Grain Boundaries in Colossal Magnetoresistive 

Films using X-ray Microdiffraction. J. Appl. Phys.. 91

(10), 7742 (2002). 

Beamline X16C

A Frenkel, O Kleifeld, S Wasserman, I Sagi. Phase 

speciation by Extended X-ray Absorption FineStructure spectroscopy . J. Chem. Phys.. 116, 9449 

(2002). 

A Frenkel, C Hills, R Nuzzo. View from the inside: 

Complexity of the atomic scale ordering in metal 

nanoparticles. J. Phys. Chem. B. 105, 12689 (2001). 

A Jokic, A Frenkel, M Vairavamurthy, P Huang. 

Birnessite catalysis of the Maillard reaction: Its 

significance in natural humification. Geophys. Res. 

Lett.. 28, 3899 (2001). 

J Rodriguez, J Hanson, A Frenkel, J Kim, M Perez. 

Experimental and Theoretical Studies on the Reaction 

of H2 with NiO: Role of O Vacancies and Mechanism 

for Oxide Reduction. J. Am. Chem. Soc.. 124 (2), 

346-354 (2002). 

Y Soh, G Aeppli, F Zimmermann, E Isaacs, A Frenkel. 

X-ray induced persistent photoconductivity in Sidoped Al0.35Ga0.65As. J. Appl. Phys.. 90, 6172 

(2001). 

Beamline X17B1

J Chen, D Weidner, M Vaughan. The Strength of 

Mg0.9Fe0.1SiO3 Perovskite at High Pressure and 

Temperature. Nature. 419, 824 (2002). 

M Croft, I Zakharchenko, Z Zhong, Y Gulak, J Hastings, 

J Hu, R Holtz, M DaSilva, T Tsakalakos. Strain Field 

and Scattered Intensity Profiling with Energy 

Dispersive X-Ray Scattering. J. Appl. Phys.. 92, 578-

586 (2002). 

B Li, R Liebermann, D Weidner. P-V-Vp-Vs-T 

Measurements on wadsleyite to 7 Gpa and 873 K: 

Implications for the 410-km seismic discontinuity. J. 

Geophys. Res.. 106 (b12), 30575-30591 (2001). 

W Mao, H Mao, A Goncharov, V Struzhkin, Q Guo, J Hu, 

J Shu, R Hemley, M Somayazulu, Y Zhao. Hydrogen 

clusters in clathrate hydrate. Science. 297, 2247-

2249 (2002). 

P Raterron, J Chen, D Weidner. A Process for the LowTemperature Olivine-Spinel Transition under quasihydrostatic stress. Geophys. Res. Lett.. 29 (10), 36-

1 to 36-4 (2002). 
Activity Report 2002 7 - 18 

H Reichert, V Bugaev, O Shchyglo, A Schˆps, Y Sikula, 

H Dosch. Strain-Induced Nonanalytic Short-Range 

Order in the Spin Glass Cu83Mn17. Phys. Rev. Lett.. 

87 (23), 236105 (2001). 

Beamline X17B2

J Chen, D Weidner, M Vaughan. In-situ x-ray 

diffraction studies of mineralogy with multi-anvil 

apparatus. Recent Research Developments in 

Mineralogy, p. 13-27, Rsearch Signpost, Trivandrum. 

(2001). 

Beamline X17C

M Croft, I Zakharchenko, Z Zhong, Y Gulak, J Hastings, 

J Hu, R Holtz, M DaSilva, T Tsakalakos. Strain Field 

and Scattered Intensity Profiling with Energy 

Dispersive X-Ray Scattering. J. Appl. Phys.. 92, 578-

586 (2002). 

H Cynn, J Klepeis, C Yoo, D Young. Osmium has the 

Lowest Experimentally Determined Compressibility. 

Phys. Rev. Lett.. 88 (13), 135701 (2002). 

D Errandonea, M Somayazulu, D Hausermann. CaWO4: 

A new high-pressure and high-temperature phase. 

Phys. Status Solidi B. 231 (1), R1-R3 (2002). 

A Kavner, T Duffy. Elasticity and strength of a natural 

ringwoodite at pressures of the Earth's transition 

zone. Geophys. Res. Lett.. 28, 2691-2694 (2001). 

H Liu, C Jin, Y Zhao. Pressure induced structural 

transitions in nanocrystalline grained selenium . 

Physica B. 315 (1-3), 210-214 (2002). 

W Mao, H Mao, A Goncharov, V Struzhkin, Q Guo, J Hu, 

J Shu, R Hemley, M Somayazulu, Y Zhao. Hydrogen 

clusters in clathrate hydrate. Science. 297, 2247-

2249 (2002). 

H Mao, R Hemley. High-pressure transformations in 

xenon hydrates. Proc Natl Acad Sci USA. 99 (1), 25-

28 (2002). 

J Patterson, A Kudryavtsev, Y Vohra. X-ray Diffraction 

and Nanoindentation Studies of Nanocrystalline 

Graphite at High Pressures. Appl. Phys. Lett.. 81

(11), 2073-2075 (2002). 

C Sanloup, H Mao, R Hemley. High-pressure 

transformations in xenon hydrates. Proc Natl Acad Sci 

USA. 99 (1), 25-28 (2002). 

C Sanloup, R Hemley, H Mao. Evidence for xenon 

silicates at high pressure and temperature. Geophys. 

Res. Lett.. 29 (18), 10.1029 (2002). 

N Velisavljevic, G Chesnut, Y Vohra, S Weir, V Malba, J 

Akella. Structural and Electrical Properties of 

Beryllium Metal at 66 GPa Studied Using Designer 

Diamond Anvils. Phys. Rev. B: Condens. Matter. 65, 

172107 (2002). 

X Xie, M Minitti, M Chen, H Mao, D Wang, J Shu, Y Fei. 

Natural high-pressure polymorph of merrillite in the 

shock veins of the Suizhou meteorite. Geochim. 

Cosmochim. Acta. 66 (13), 2439-2444 (2002). 

Beamline X18A

Y Glanville, D Narehood, P Sokol, A Amma, T Mallouk. 

Preparation and Synthesis of Ag2Se Nanowires 

Produced by Template Directed Synthesis. J Mater. 

Chem.. 12 (8), 2433 (2002). 

D Silva, P Sokol, S Ehrlich. Mobility Transition of Solid 

Rare Gases in Confined Environments. Phys. Rev. 

Lett.. 88 (15), 155701-1 (2002). 

X Sun, X Yang, M Balasubramanian, J McBreen, Y Xia, 

T Sakai. In situ Investigation of Phase Transitions of 

Li1+yMn2O4 Spinel during Li-Ion Extraction and 

Insertion. J. Electrochem. Soc.. 149, A842 (2002). 

Z Wu, S Ehrlich, B Matthies, K Herwig, P Dai, U 

Volkmann, F Hansen, H Taub. Growth of n-alkane 

films on a single-crystal substrate. Chem. Phys. Lett.. 

348, 168-174 (2001). 

Z Wu. Diffraction Studies of Structure and Growth of 

Films Adsorbed on the Ag(111) Surface. Ph.D. Thesis. 

University of Missouri - Columbia, Columbia. (1997). 

X Yang, j McBreen, W Yoon, C Grey. Crystal Structure 

Changes of LiMn0.5Ni0.5O2 Cathode Materials during 

Charge and Discharge Studied by Synchrotron Based 

In Situ XRD. Electrochem. Commun.. 4, 649 (2002). 

W Yoon, Y Paik, X Yang, M Balasubramanian, J 

McBreen, C Grey. Investigation of the Local Structure 

of the LiNi0.5Mn0.5O2 Cathode Material during 

Electrochemical Cycling by X-Ray Absorption and 

NMR Spectroscopy. Electrochem. Solid-State Lett.. 5, 

A263 (2002). 

Y Zhang, S Ehrlich, R Colella, M Kopecky, M Widom. Xray Diffuse Scattering in Icosahedral Quasicrystal AlPd-Mn. Phys. Rev. B. 66, 104202 (2002). 

Beamline X18B

F Alamgir, H Jain, G Hug, R Schwarz. EXAFS and 

EXELFS Study of the Structure of Pd-Ni-P Bulk 

Metallic Glasses. Materials Research Society, Vol 644, 

p. L2.4.1, (2001). 

A Ankudinov, J Rehr, J Low, S Bare. Sensitivity of Pt xray absorption near edge structure to the morphology 

of small Pt clusters. J. Chem. Phys.. 116 (5), 1911-

1919 (2002). 

G Chen, S Bare, T Mallouk. Development of supported 

bifunctional electrocatalysts for unitized regenerative 

fuel cells. J. Electrochem. Soc.. 149 (8), A1092-

A1099 (2002). 

M Farmer, L Boatner, B Chakoumakos, C Rawn, J 

Richardson, S Khalid. Polymorphism and a phase 

transition in K3Yb(PO4)2. International Union of 

Crystallography, Geneva, Switzerland, Vol XIX, p. x, 

sponsored by International Union of Crystallography. 

(2002). 

E Ghabbour, A Scheinost, G Davies. XAFS Studies of 

Cobalt(ll) Binding by Peat, Plant and Soil Derived 

Solid Humic Acids. The 20th Anniversary Conference 

of the International Humic Substances Society , Vol 

IHSS 11, p. 277-282, sponsored by International 

Humic Substances Society . (2002). 

E Ghabbour, A Scheinost, G Davies. XAFS Studies of 

Cobalt(ll) Binding by Peat, Plant and Soil Derived 

Solid Humic Acids. Synchrotron Environmental 

Science-II Conference, May 6-8, 2002 , Vol II, p. 40, 

sponsored by Advanced Photon Source. (2002). 

F Huggins, G Huffman, A Kolker, S Mroczkowski, C 

Palmer, R Finkelman. Combined application of XAFS 

spectroscopy and sequential leaching for 

determination of arsenic speciation in coal. Energ. 

Fuel. 16 (5), 1167-1172 (2002). 
7 - 19 Publications

F Huggins, G Huffman. X-ray absorption fine structure 

(XAFS) spectroscopic characterization of emissions 

from combustion of fossil fuels. Int. J. Soc. Mat. Eng. 

Res.. 10 (1), 1-13 (2002). 

G Jacobs, P Patterson, Y Zhang, T Das, J Li, B Davis. 

Fischer-Tropsch synthesis: Deactivation of Noble 

Metal Promoted Co/Al2O3 Catalysts. Appl. Catal. A. 

233, 215-226 (2002). 

M Olivella, J Palacios, A Vairavamurthy, J del Rio, F de 

las Heras. A Study of Sulfur Functionalities in Fossil 

Fuels Using Destructive (ASTM and Py-GC-MS) and 

non-destructive (SEM-EDX, XANES, and XPS) 

Techniques. Fuel. 81, 405-411 (2002). 

J Rakovan, R Reeder, E Elzinga, D Cherniak, C Tait, D 

Morris. Structural Characterization of U(VI) in Apatite 

by X-ray Absorption Spectroscopy. Environ. Sci. 

Tech.. 36 (14), 3114-3117 (2002). 

K Ramanujschary, S Lofland, W McCarroll, T Emge, M 

Greenblatt, M Croft. Substitutional Effects of 3d 

Transition Metals on the Magnetic and Structural 

Properties of Quasi-Two-Dimensional La5Mo4O16. J. 

Solid State Chem.. 164, 60-70 (2002). 

J Rehr, J Low, S Bare. Theoretical interpretation of 

XAFS and XANES in Pt clusters. Top. Catal.. 18 (1-2), 

3-7 (2002). 

J Shearer, R Scarrow, J Kovacs. Synthetic Models For 

the CysteinateñLigated NonñHeme Iron Enzyme 

Superoxide Reductase: Observation and Structural 

Characterization by XAS of an Fe(III)-OOH 

Intermediate. J. Am. Chem. Soc.. 124 (39), 11709-

11717 (2002). 

T Shoji, F Huggins, G Huffman, W Linak, C Miller. XAFS 

Spectroscopy Analysis of Selected Elements in Fine 

Particulate Matter Derived from Coal Combustion. 

Energ. Fuel. 16 (2), 325-329 (2002). 

G Veith, R Chen, G Popov, M Greenblatt, M Croft, I 

Nowik. Electronic, Magnetic and Magnetoresistance 

Properties of the n = 2 Ruddlesden-Popper Phases 

Sr3Fe2-xCoxO7-d (0.25 < x < 1.75). J. Solid State 

Chem.. 166, 292-304 (2002). 

R Viswanathan, G Hou, R Liu, S Bare, F Modica, G 

Mickelson, C Segre, N Leyarovska, E Smotkin. In situ 

XANES of carbon-supported Pt-Ru anode 

electrocatalyst for reformate-air polymer electrolyte 

fule cells. J. Phys. Chem. B. 106 (13), 3458-3465 

(2002). 

W Yoon, Y Paik, X Yang, M Balasubramanian, J 

McBreen, C Grey. Investigation of the Local Structure 

of the LiNi0.5Mn0.5O2 Cathode Material during 

Electrochemical Cycling by X-Ray Absorption and 

NMR Spectroscopy. Electrochem. Solid-State Lett.. 5, 

A263 (2002). 

Beamline X19A

S Beauchemin, D Hesterberg, M Beauchemin. Principal 

component analysis approach for modeling sulfur KXANES spectra of humic acids. Soil Sci. Soc. Am. J.. 

66, 83-91 (2002). 

B Bostick, M Vairavamurthy, K Karthikeyan, J 

Chorover. Cesium Adsorption on Clay Minerals: An 

EXAFS Spectroscopic Investigation. Environ. Sci. 

Tech.. 36, 2670-2676 (2002). 

A Cady, R Pindak, W Caliebe, P Barois, W Weissflog, H 

Nguyen, C Huang. Resonant x-ray scattering studies 

of the B2 phase formed by bent-core molecules. Liq. 

Cryst.. 29 (8), 1101-1104 (2002). 

F Huggins, G Huffman, A Kolker, S Mroczkowski, C 

Palmer, R Finkelman. Combined application of XAFS 

spectroscopy and sequential leaching for 

determination of arsenic speciation in coal. Energ. 

Fuel. 16 (5), 1167-1172 (2002). 

F Huggins, G Huffman. X-ray absorption fine structure 

(XAFS) spectroscopic characterization of emissions 

from combustion of fossil fuels. Int. J. Soc. Mat. Eng. 

Res.. 10 (1), 1-13 (2002). 

C Martinez, M McBride, M Kandianis, J Duxbury, S 

Yoon, W Bleam. Zinc-sulfur and cadmium-sulfur 

association in metalliferous peats: evidence from 

spectroscopy, distribution coefficients, and 

phytoavailability. Environ. Sci. Tech.. 36 (17), 3683-

3689 (2002). 

L Matkin, S Watson, H Gleeson, P Cluzeau, P Barois, R 

Pindak, J Pitney, A Cady, C Huang, et al. The 

interlayer structures of the chiral smectic liquid 

crystal phases revealed by x-ray resonant scattering. 

Phys. Rev. E. 65, 41705-41714 (2002). 

H Oh, J Yang, C Costello, Y Wang, S Bare, H Kung, M 

Kung. Selective catalytic oxidation of CO: Effect of 

chloride on supported Au catalysts. J. Catal.. 210

(2), 375-386 (2002). 

M Olivella, J Rio, J Palacios, A Vairavamurthy, F de las 

Heras. Characterization of humic acid from leonardite 

coal: an integrated study of Py-GC-MS, XPS and 

XANES techniques. J. Anal. Appl. Pyrolysis. 63, 59-68 

(2002). 

M Olivella, J Palacios, A Vairavamurthy, J del Rio, F de 

las Heras. A Study of Sulfur Functionalities in Fossil 

Fuels Using Destructive (ASTM and Py-GC-MS) and 

non-destructive (SEM-EDX, XANES, and XPS) 

Techniques. Fuel. 81, 405-411 (2002). 

D Peak, J Sims, D Sparks. Solid State Speciation of 

Natural and Alum-amended Polutry Litter using 

XANES Spectroscopy. Environ. Sci. Tech.. 36, 4253-

4261 (2002). 

J Qian. Mercury species in environmental samples 

studied by spectroscopic methods. Ph.D. Thesis. 

Department of Forest Ecology, Swedish University of 

Agricultural Sciences, UmeÂ. (2001). 

K Ramanujschary, S Lofland, W McCarroll, T Emge, M 

Greenblatt, M Croft. Substitutional Effects of 3d 

Transition Metals on the Magnetic and Structural 

Properties of Quasi-Two-Dimensional La5Mo4O16. J. 

Solid State Chem.. 164, 60-70 (2002). 

J Rodriguez, J Hrbek. Interaction of sulphur with 

bimetallic surfaces: Effects of Structural, electronic 

and chemical properties. The Chemical Physics of 

Solid Surfaces: Surface Alloys and Alloy Surfaces, p. 

374, Elsevier, Amsterdam. (2002). 

J Rodriguez, T Jirsak, L Gonzalez, J Evans, M Perez, A 

Maiti. Reaction of SO2 with pure and metal-doped 

MgO: Basic principles for the cleavage of S-O bonds. 

J. Chem. Phys.. 115, 10914 (2001). 

J Rodriguez. Environmental Catalysis and The 

Chemistry of SO2 on Oxide Surfaces. Ciencia. 9, 139 

(2001). 
Activity Report 2002 7 - 20 

T Shoji, F Huggins, G Huffman, W Linak, C Miller. XAFS 

Spectroscopy Analysis of Selected Elements in Fine 

Particulate Matter Derived from Coal Combustion. 

Energ. Fuel. 16 (2), 325-329 (2002). 

X Sun, H Lee, X Yang, J McBreen. Synthesis and Study 

of New Cyclic Boronate Additives for Lithium Battery 

Electrolytes. J. Electrochem. Soc.. 149, A1460 

(2002). 

J Tetenbaum, L Miller. A new spectroscopic approach to 

examining the role of disulfide bonds in the Structure 

and Unfolding of Soybean Trypsin Inhibitor. 

Biochemistry. 40, 12215-19 (2001). 

G Veith, R Chen, G Popov, M Greenblatt, M Croft, I 

Nowik. Electronic, Magnetic and Magnetoresistance 

Properties of the n = 2 Ruddlesden-Popper Phases 

Sr3Fe2-xCoxO7-d (0.25 < x < 1.75). J. Solid State 

Chem.. 166, 292-304 (2002). 

Beamline X19C

M Dudley, W Vetter, P Neudeck. Polytype Identification 

in Heteroepitaxial 3C-SiC Grown on 4H-SiC Mesas 

Using Synchrotron White Beam X-ray Topography. J. 

Cryst. Growth. 240, 22 (2002). 

M Dudley, W Vetter, P Neudeck, J Powell. Polytype 

Identification and Mapping in Hetroepitaxial Growth 

of 3C on Atomically Flat 4H-SiC Mesas Using 

Synchrotron White Beam X-ray Topography. 

International Conference on Silicon Carbide and 

Related Materials 2001, Vol 389-393, p. 391-394, 

sponsored by Science & Technology Promotion 

Foundation of Ibaraki (et al). (2002). 

S Ha, W Vetter, M Dudley, M Skowronski. A Simple 

Mapping Method for Elementary Screw Dislocations in 

Homoepitaxial SiC Layersî, . International Conference 

on Silicon Carbide and Related Materials 2001, Vol 

389-393, p. 443-446, sponsored by Science & 

Technology Promotion Foundation of Ibaraki (et al). 

(2002). 

S Ha, M Skowronski, W Vetter, M Dudley. Basal Plane 

Slip and Formation of Mixed-Tilt Boundaries, in 

Sublimation-Grown Hexagonal Polytype Silicon 

Carbide Single Crystals. J. Appl. Phys.. 92, 778-785 

(2002). 

M Hollingsworth, M Brown, M Dudley, H Chung, M 

Peterson, A Hillier. Template Effects, Asymmetry and 

Twinning in Helical Inclusion Compounds. Angew. 

Chem. Int. Ed.. 41, 965-969 (2002). 

M Li, M Schlossman. X-ray scattering of thin liquid 

films: Beyond the harmonic approximation. Phys. 

Rev. E. 65, 061608 (2002). 

D Li, B Yang, S Rice. Structure of the liquid-vapor 

interface of a dilute ternary alloy: Pb and Sn in Ga. 

Phys. Rev. B: Condens. Matter. 65 (22), 224202 

(2002). 

M Li, A Tikhonov, M Schlossman. An X-ray diffuse 

scattering study of domains in F(CF2)10(CH2)2OH 

monolayers at the hexane-water interface. Europhys. 

Lett.. 58 (1), 80 (2002). 

P Neudeck, J Powell, A Trunek, D Spry, G Beheim, E 

Benavage, P Abel, W Vetter, M Dudley. Homoepitaxial 

ìWeb Growthî of SiC to Terminate c-axis Screw 

Dislocations and Enlarge Step-Free Surfaces. 

International Conference on Silicon Carbide and 

Related Materials 2001, Vol 389-393, p. 251-254, 

sponsored by Science & Technology Promotion 

Foundation of Ibaraki (et al). (2002). 

P Neudeck, J Powell, A Trunek, X Huang, M Dudley. 

Growth of defect-Free 3C-SiC on 4H- and 6H-SiC 

Mesas Using Step-Free Surface Heteroepitaxy. 

International Conference on Silicon Carbide and 

Related Materials 2001, Vol 389-393, p. 311-314, 

sponsored by Science & Technology Promotion 

Foundation of Ibaraki (et al). (2002). 

P Neudeck, J Powell, G Beheim, E Benavage, P Abel, A 

Trunek, D Spry, M Dudley, W Vetter. Enlargement of 

Step-Free SiC Surfaces by Homoepitaxial WebGrowth of Thin SiC Cantilevers. J. Appl. Phys.. 92, 

2391-2400 (2002). 

B Raghothamachar. Synchrotron white beam x-ray 

characterization of growth defects in bulk compound 

semiconductors. Ph.D. Thesis. State Univ. of New 

York at Stony Brook, Stony Brook. (2001). 

B Raghothamachar, W Vetter, M Dudley, R Dalmau, R 

Schlesser, Z Sitar, E Michaels, J Kolis. Synchrotron 

White Beam Topography Characterization of Physical 

Vapor Transport Grown AlN and Ammonothermal 

GaN. J. Cryst. Growth. 246, 271-280 (2002). 

J Rojo, L Schowalter, G Slack, K Morgan, J Barani, S 

Schujman, S Biswas, B Raghothamachar, M Dudley, 

et al.. Progress in the Preparation of Aluminum 

Nitride Substrates from Bulk Crystals. Materials 

Research Society Spring Meeting 2002, Vol 722, p. 5-

13, sponsored by Materials Research Society. (2002). 

E Sanchez, S Ha, J Grim, M Skowronski, W Vetter, M 

Dudley, R Bertke, W Mitchel. Assessment of Polishing 

Related Surface Damage in Silicon Carbide. J. 

Electrochem. Soc.. 149, G131 (2001). 

E Sanchez, J Liu, M De Graef, M Skowronski, W Vetter, 

M Dudley. Nucleation of Threading Dislocations in 

Sublimation Grown Silicon Carbide. J. Appl. Phys.. 

91, 1143-1148 (2002). 

M Schlossman. Liquid-liquid interfaces: studied by Xray and neutron scattering. Diabetes. 7, 235-243 

(2002). 

Y Seo, K Kim, K Shin, H White, M Rafailovich, J 

Sokolov, B Lin, H Kim, C Zhang, et al. Morphology of 

Ampiphilic Gold/Dendrimer Nanocomposite 

Monolayers. Langmuir. 18, 5927-5932 (2002). 

M Skowronski, J Liu, W Vetter, M Dudley, C Hallin, H 

Lendenmann. Recombination-Enhanced Defect 

Motion in Forward-Biased 4H-SiC p-n Diodes. J. Appl. 

Phys.. 92, 4699-4704 (2002). 

B Skromme, K Palle, C Poweleit, L Bryant, W Vetter, M 

Dudley, K Moore , T Gehoski. Oxidation-Induced 

Crystallographic Transformation in Heavily N-Doped 

4H-SiC Wafers. International Conference on Silicon 

Carbide and Related Materials 2001, Vol 389-393, p. 

455-458, sponsored by Science & Technology 

Promotion Foundation of Ibaraki (et al). (2002). 

W Vetter, D Gallagher, M Dudley. Synchrotron Whitebeam X-ray Topography of Ribonuclease S Crystals. 

Acta Cryst. D. D58, 579-584 (2002). 
7 - 21 Publications

W Vetter, H Totsuka, M Dudley, B Kahr. The Perfection 

and Defect Structure of Organic Hourglass Inclusion 

K2SO4 Crystals. J. Cryst. Growth. 241, 498-506 

(2002). 

E Vetter, M Dudley. Partial Dislocations in the X-ray 

Topography of As-Grown Hexagonal Silicon Carbide 

Crystals. Mater. Sci. Eng. A. B87, 173-177 (2001). 

M Wijesundara, G Zajac, E Fuoco, L Hanley. Aging of 

Fluorocarbon Thin Films Deposited on Polystyrene 

from Hyperthermal C3F5+ and CF3+ Ion Beams. J. 

Adhes. Sci. Technol.. 15, 599-612 (2001). 

Beamline X20A

R Christianson, Y Wang, S LaMarra, R Birgeneau, V 

Kiryukhin, T Masuda, I Tsukada, K Uchinokura, B 

Keimer. X-ray Scattering Study of the 

Incommensurate Phase in Mg-Doped CuGeO3 . Phys. 

Rev. B: Condens. Matter. 66, 174105 (2002). 

M Doerner, X Bian, M Madison, K Tang, Q Peng, A 

Polcyn, T Arnoldussen, M Toney, M Mirzamaani, et 

al.. Demonstration of 35 Gbit/in2 Media on a Glass 

Substrate. IEEE Trans. Magn.. 37 (2), 1052 (2001). 

J Hanan, E ‹st ̧ndag, D Dragoi, I Noyan, D Haeffner, P 

Lee. Residual Stresses in Ti-SiC Composites. Adv. XRay Anal.. 44, 156-161 (2001). 

J Hanan. Damage Evolution in Uniaxial SiC Fiber 

Reinforced Ti Matrix Composites. Ph.D. Thesis. 

California Institute of Technology, Pasadena. (2002). 

J Hanan, C Aydiner, E ‹st ̧ndag, G Swift, S Kaldor, I 

Noyan. Characterization of Fiber/Matrix Interfaces 

Using X-Ray Microtopography. Mater. Sci. Forum. 

404-407, 919-924 (2001). 

S Kaldor. X-ray Microbeam Studies of Anticlastic 

Curvature in Elastically Bent Silicon Beams and 

Plates. Ph.D. Thesis. Columbia University, New York. 

(2002). 

S Kaldor, I Noyan. Differentiating between elastically 

bent rectangular beams and plates. Appl. Phys. Lett.. 

80 (13), 2284-2286 (2002). 

S Kiselev, V Khmelenko, D Lee, V Kiryukhin, R Boltnev, 

E Gordon, B Keimer. Structural studies of impurityhelium solids. Phys. Rev. B. 65, 024517 (2001). 

S Kiselev, V Khmelenko, D Lee, V Kiryukhin, R Boltnev, 

E Gordon, B Keimer. X-ray Studies of Structural 

Changes of Impuroty-Helium Solids. J. Low Temp. 

Phys.. 126, 235 (2002). 

L Oblonsky, A Davenport, M Ryan, M Toney. In-situ 

XRD Study of the Passive Film that Forms on Iron in 

Borate Buffer. Proceedings of 8th International 

Conference on Passivity of Metals and 

Semiconductors 1999, Jasper, Canada, p. 173-179, 

(2001). 

A Ozcan, K Ludwig, P Rebbi, C Cabral, Jr., C Lavoie, J 

Harper. Texture of TiSi2 Thin Films on Si(001). J. 

Appl. Phys.. 92, 5011 (2002). 

S Park, R Leheny, R Birgeneau, J Gallani, C Garland, G 

Iannacchione. Hydrogen-bonded silica gels dispersed 

in a smectic liquid crystal: A random field XY system. 

Phys. Rev. E. 65 (5), 050703(R) (2002). 

M Ryan, M Toney, L Oblonsky, A Davenport. The 

Structure of the Passive Film that Forms on Iron in 

Aqueous Environments. Solid-Liquid Interface 

Theory, p. 85, American Chemical Society, 

Washington. (2001). 

Beamline X20C

J Chun, P Desjardins, C Lavoie, I Petrov, C Cabral, Jr., 

J Greene. Interfacial Reaction Pathways and Kinetics 

During Annealing of 111-textured Al/TiN Bilayers: A 

Synchrotron X-ray Diffraction and Transmission . J. 

Vac. Sci. Technol., A. 19, 2207 (2001). 

F D'Heurle, S Zhang, C Lavoie, P Gas, C Cabral, Jr., J 

Harper. Formation of C54 TiSi2: Effect of Niobium 

Addition on the Apparent Activation Energy. J. Appl. 

Phys.. 90 (11), 6409 (2001). 

M Doerner, X Bian, M Madison, K Tang, Q Peng, A 

Polcyn, T Arnoldussen, M Toney, M Mirzamaani, et 

al.. Demonstration of 35 Gbit/in2 Media on a Glass 

Substrate. IEEE Trans. Magn.. 37 (2), 1052 (2001). 

H Ishibashi, T Yoo, Y Hor, A Borissov, Y Horibe, P 

Radaelli, S Cheong, V Kiryukhin. X-ray-induced 

Disordering of the Dimerization Pattern and Apparent 

Low-temperature Enhancement of Lattice Symmetry 

in Spinel CuIr2S4. Phys. Rev. B: Condens. Matter. 

66, 144424 (2002). 

S Kaldor. X-ray Microbeam Studies of Anticlastic 

Curvature in Elastically Bent Silicon Beams and 

Plates. Ph.D. Thesis. Columbia University, New York. 

(2002). 

S Kaldor, I Noyan. Differentiating between elastically 

bent rectangular beams and plates. Appl. Phys. Lett.. 

80 (13), 2284-2286 (2002). 

H Kim, C Cabral, Jr., C Lavoie, S Rossnagel. Diffusion 

Barrier Properties of Transition Metal Thin Films 

Grown by Plasma Enhanced Atomic Layer Deposition. 

J. Vac. Sci. Technol., B. 20 (4), 1321 (2002). 

V Kiryukhin, T Koo, A Borissov, Y Kim, S Nelson, J Hill, 

D Gibbs, S Cheong. Common Features of nanoscale 

structural correlations in magnetoresistive 

manganites with a ferromagnetic low-temperature 

state. Phys. Rev. B. 65, 094421 (2002). 

C Lavoie, C Cabral, Jr., F D'Heurle, J Jordan-Sweet, J 

Harper. Effects of Alloying Elements on Cobalt Silicide 

Formation. J. Electron. Mater.. 31 (6), 597 (2002). 

G Lucadamo, K Barmak, C Lavoie, C Cabral, Jr., C 

Michaelsen. Metastable and Equilibrium Phase 

Formation in Sputter Deposited Ti/Al Multilayer Films. 

J. Appl. Phys.. 91 (12), 9575 (2002). 

R Martel, V Derycke, C Lavoie, J Appenzeller, K Chan, J 

Tersoff, P Avouris. Ambipolar Electrical Transport in 

Semiconducting Single-wall Carbon Nanotubes. Phys. 

Rev. Lett.. 87, 256805 (2001). 

L Oblonsky, A Davenport, M Ryan, M Toney. In-situ 

XRD Study of the Passive Film that Forms on Iron in 

Borate Buffer. Proceedings of 8th International 

Conference on Passivity of Metals and 

Semiconductors 1999, Jasper, Canada, p. 173-179, 

(2001). 

A Ozcan, K Ludwig, P Rebbi, C Cabral, Jr., C Lavoie, J 

Harper. Texture of TiSi2 Thin Films on Si(001). J. 

Appl. Phys.. 92, 5011 (2002). 

A Ozcan, K Ludwig, Jr., C Lavoie, C Cabral, Jr., J 

Harper, R Bradley. Nucleation and Growth Kinetics of 

Preferred C54 TiSi2 Orientations: Time-resolved Xray Diffraction Measurements. J. Appl. Phys.. 92, 

5189 (2002). 
Activity Report 2002 7 - 22 

A Ozcan, K Ludwig, Jr., C Cabral, Jr., J Harper. In Situ 

Studies of Silicide Formation in TiTa Bilayer Thin 

Films on Poly-Silicon. Materials Research Society 

Symposium, Vol 721, p. 1, sponsored by Materials 

Research Society. (2002). 

S Park, R Leheny, R Birgeneau, J Gallani, C Garland, G 

Iannacchione. Hydrogen-bonded silica gels dispersed 

in a smectic liquid crystal: A random field XY system. 

Phys. Rev. E. 65 (5), 050703(R) (2002). 

M Ryan, M Toney, L Oblonsky, A Davenport. The 

Structure of the Passive Film that Forms on Iron in 

Aqueous Environments. Solid-Liquid Interface 

Theory, p. 85, American Chemical Society, 

Washington. (2001). 

Beamline X21

K Hamalainen, S Manninen. Resonant and NonResonant Inelastic X-Ray Scattering. J. Phys.: 

Condens. Matter. 13, 7539 (2001). 

H Hayashi, Y Udagawa, W Caliebe, C Kao. Hidden 

Electronic State of CuO Revealed by Resonant 

Inelastic X-ray Scattering. Phys. Rev. B. 66, 033105-

1 (2002). 

S Huotari, K Hamalainen, J Laukkanen, A Soininen, S 

Manninen, C Kao, T Buslaps, M Mezouar, H Kao. High 

Pressure Compton Scattering. AIRAPT-17, 

International Conference on Science and Technology 

of High Pressure, Vol 2, p. 1017, (2000). 

J Soininen, K Hamalainen, W Caliebe, C Kao, E Shirley. 

Core Hole - Electron Interaction in X-Ray Raman 

Scattering. J. Phys.: Condens. Matter. 13, 8039 

(2001). 

J Soininen, K Hamalainen, S Manninen. Final-state 

Electron-electron Interaction in Compton Scattering. 

Phys. Rev. B: Condens. Matter. 64 (1-7), 125116 

(2001). 

L Yang, H Huang. Observation of a Membrane Fusion 

Intermediate Structure. Science. 297 (5588), 1877-

1879 (2002). 

Beamline X22A

A Baptiste, A Gibaud, J Bardeau, K Wen, R Maoz, J 

Sagiv, B Ocko. X-Ray, Micro-Raman, and Infrared 

Spectroscopy Structural Characterization of SelfAssembled Multilayer Silane Films with Variable 

Numbers of Stacked Layers. Langmuir. 18 (10), 

3916-3922 (2002). 

J DeVilbiss, J Wang, B Ocko, K Tamura, R Adzic, I 

Vartanyants, I Robinson. Time Response of the Thin 

Layer Electrochemical Cell Used for in situ X-ray 

Diffraction. Electrochim. Acta. 47, 3057-3064 

(2002). 

E DiMasi, J Fossum, T Gog, C Venkataraman. 

Orientational order in gravity dispersed clay colloids: 

a synchrotron x-ray scattering study of Na 

fluorohectorite suspensions. Phys. Rev. E. 64, 61704 

(2001). 

K Tamura, B Ocko, J Wang, R Adzic. Structure of Active 

Adlayers on Bimetallic Surfaces: Oxygen Reduction 

on Au(111) with Bi Adlayers. J. Phys. Chem. B. 106, 

3896-3901 (2002). 

Z Ye, B Noheda, M Dong, D Cox, G Shirane. Monoclinic 

phase in the relaxor-based piezoelectric/ferroelectric 

Pb(Mg1/3Nb2/3)O3-PTiO3. Phys. Rev. B: Condens. 

Matter. 64, 184114 (2001). 

Beamline X22B

E DiMasi, H Tostmann. Surface Induced Order in Liquid 

Metal Alloys. Synch. Rad. News. 12, 41 (1999). 

E DiMasi, L Gower. Synchrotron X-ray Observations of 

a Monolayer Template for Mineralization. Materials 

Research Society Fall Meeting 2001, Vol 711, p. 301, 

sponsored by Materials Research Society. (2002). 

O Gang, M Fukuto, P Huber, P Pershan. Wetting of 

Hydrocarbon Liquid Surfaces by Fluorocarbon Vapor: 

A Microscopic Study. Coll. Surf. A. 206, 293 (2002). 

P Huber, O Shpyrko, P Pershan, B Ocko, E DiMasi, W 

Press. Tetra Point Wetting at the Free Surface of 

Liquid Ga-Bi. Phys. Rev. Lett.. 89, 35502 (2002). 

P Huber, O Shpyrko, P Pershan, H Tostmann, E DiMasi, 

B Ocko, M Deutsch. Wetting behavior at the free 

surface of a liquid gallium-bismuth alloy: an x-ray 

reflectivity study close to the bulk monotectic point. 

Coll. Surf. A. 206 (1-3), 515-520 (2002). 

T Koo, V Kiryukhin, P Sharma, J Hill, S Cheong. 

Magnetic-field-induced collapse of charge-ordered 

nanoclusters and the colossal magnetoresistance 

effect in Nd0.3Sr0.3MnO3. Phys. Rev. B. 64, 220405 

(2001). 

W Pao, M Stetzer, P Heiney, W Cho, V Percec. X-ray 

Reflectivity Study of Langmuir Films of Amphiphilic 

Monodendrons. J. Phys. Chem. B. 105, 2170-2176 

(2001). 

T Seydel, M Tolan, B Ocko, O Seeck, R Weber, E 

DiMasi, W Press. Freezing of capillary waves at the 

glass transition. Phys. Rev. B. 65 (18), 184207 

(2002). 

K Shin, Y Zhang, H White, M Rafailovich, J Sokolov, D 

Peiffer. Organoclay Nanoplatelets at the Air/water 

Interface. Materials Research Society, Vol KK8.4 , 

(2001). 

E Sloutskin, E Sirota, H Kraack, O Gang, A Doerr, B 

Ocko, M Deutsch. Surface and bulk phase behavior of 

dry and hydrated tetradecanol:octadecanol alcohol 

mixtures. J. Chem. Phys.. 116 (18), 8056-8066 

(2002). 

E Sloutskin, H Kraack, B Ocko, J Ellmann, M Moller, P 

Lo Nostro, M Deutsch. Thermal Expansion of SurfaceFrozen Monolayers of Semifluorinated Alkanes. 

Langmuir. 18, 1963-1967 (2002). 

Beamline X22C

A Baddorf, V Jahns, D Zehner, H Zajonz, D Gibbs. 

Relaxation and thermal expansion of Ru(0001) 

between 300 and 1870 K. Surf. Sci.. 498, 74 (2002). 

D Gibbs, J Hill, C Vettier. New directions in x-ray 

magnetic scattering. Third Generation Hard X-ray 

Synchrotron Radiation Sources: Source Properties, 

Optics and Experimental Techniques, p. 267-310, J. 

Wiley & Sons, Inc., New York. (2002). 
7 - 23 Publications

V Kiryukhin, T Koo, A Borissov, Y Kim, S Nelson, J Hill, 

D Gibbs, S Cheong. Common Features of nanoscale 

structural correlations in magnetoresistive 

manganites with a ferromagnetic low-temperature 

state. Phys. Rev. B. 65, 094421 (2002). 

U Klemradt, M Aspelmeyer, H Abe, L Wood, S Moss, E 

DiMasi, J Peisl. Premonitory Martensitic Surface Relief 

via Novel X-ray Diffuse and Laser Light Reflectivity 

from the (001) Surface of a Ni63Al37 Single Crystal. 

Materials Research Society Fall Meeting 1999, Vol 

580, p. 293, sponsored by Materials Research 

Society. (2000). 

Beamline X23A2

F Alamgir, H Jain, G Hug, R Schwarz. EXAFS and 

EXELFS Study of the Structure of Pd-Ni-P Bulk 

Metallic Glasses. Materials Research Society, Vol 644, 

p. L2.4.1, (2001). 

S Calvin. Relationship Between Electron Delocalization 

and Asymmetry of the Pair Distribution Function as 

Determined by X-Ray Absorption Spectroscopy. Ph.D. 

Thesis. City University of New York, New York. 

(2001). 

M Duff, J Coughlin, D Hunter. Uranium Co-precipitation 

with Iron Oxide Minerals. Geochim. Cosmochim. Acta. 

66 (20), 3533-3547 (2002). 

D McKeown, I Muller, K Matlack, I Pegg. X-ray 

absorption studies of vanadium valence and local 

environment in borosilicate waste glasses using 

vanadium sulfide, silicate, and oxide standards. J. 

Non-Cryst. Solids. 298, 160-175 (2002). 

J Rose, M Cortalezzi-Fidalgo, S Moustier, C Magnetto, C 

Jones, A Barron, M Wiesner, J Bottero. Synthesis and 

Characterization of Carboxylate-FeOOH Nanoparticles 

(Ferroxanes) and Ferroxane-Derigved Ceramics. 

Chem. Mater.. 14 (2), 621-628 (2002). 

A Sahiner, S Novak, J Woicik, J Liu, V Krishnamoorty. 

Determining the Ratio of the Precipitated versus 

Substituted Arsenic by XAFS and SIMS in Heavy Dose 

Arsenic Implants in Silicon. Materials Research 

Society Spring Meeting 2001, Vol 669, p. J5.8.1-7, 

sponsored by Materials Research Society. (2001). 

M Sahiner, S Novak, J Woicik, Y Takamura, P Griffin, J 

Plummer. The Local Structure of Antimony in High 

Dose Antimony Implants in Silicon by XAFS and 

SIMS. MRS Spring 2002, Vol 717, p. C3.6.1-7, 

sponsored by Materials Research Society. (2002). 

Beamline X23B

S Calvin. Relationship Between Electron Delocalization 

and Asymmetry of the Pair Distribution Function as 

Determined by X-Ray Absorption Spectroscopy. Ph.D. 

Thesis. City University of New York, New York. 

(2001). 

L Dieng, A Ignatov, T Tyson, M Croft, F Dogan, C Kim, 

J Woicik, J Grow. Observation of changes in the 

atomic and electronic structure of single-crystal 

YBa2Cu3O6.6 accompaying bromination. Phys. Rev. 

B: Condens. Matter. 66, 014508 (2002). 

G Evmenenko, C Yu, J Kmetko, P Dutta. Density 

Anomalies in Thin Liquid Films of Hydride Functional 

Siloxanes. Langmuir. 18, 5468-5472 (2002). 

J Malinsky, J Veinot, G Jabbour, S Shaheen, J 

Andersen, P Lee, A Richter, A Burin, M Ratner, et al. 

Nanometer-scale Dielectric Self-assembly Process for 

Anode Modification in Organic Light-Emitting Diodes. 

Consequences for Charge Injection and Enhanced 

Luminous Efficiency. Chem. Mater.. 14, 3054-3065 

(2002). 

P Pfalzer, J Will, A Nateprov, M Klemm, V Eyert, S 

Horn, A Frenkel, S Calvin, M denBoer. Local 

Symmetry Breaking in Paramagnetic Insulating 

(Al,V)2O3. Phys. Rev. B: Condens. Matter. 66, 

085119 (2002). 

B Ravel, M Raphael, V Harris, Q Huang. EXAFS and 

Neutron Diffraction Studies of the Heusler Alloy 

Co2MnSi. Phys. Rev. B. 65 (18), 184431 (2002). 

B Ravel, V Harris, E Carpenter. Oxidation of iron in 

iron/gold core/shell nanoparticles. J. Appl. Phys.. 91

(10), 8195 (2002). 

M van der Boom, G Evmenenko, P Dutta, T Marks. 

Refractive Index Tuning of Siloxane-Based ElectroOptic Self-Assembled Superlattices. Advanced 

Materials. 11 (5), 393-397 (2001). 

M van der Boom, P Zhu, G Evmenenko, J Malinsky, W 

Lin, P Dutta, T Marks. Nanoscale Consecutive SelfAssembly of Thin-Film Molecular Materials for 

Electrooptic Switching. Chemical Streamlining and 

Ultrahigh Response Chromophores. Langmuir. 18, 

3703-3704 (2002). 

M van der Boom, G Evmenenko, P Dutta, T Marks. 

Layer-by-layer self-assembly of intrisically acentric 

organic superlattices - characterization of the 

chromophore deposition step. Polym. Mater. Sci. 

Eng.. 87, 375-376 (2002). 

Beamline X24A

T Jach, E Landree. Grazing Incidence X-Ray 

Photoelectron Spectroscopy: A Method to Study Gate 

Dielectric Films on Si. International Symposium on 

Practical Surface Analysis, Vol 9, p. 339-343, 

sponsored by Surface Analysis Society of Japan. 

(2002). 

C Kim, M Bedzyk, E Nelson, J Woicik, L Berman. Sitespecific valence-band photoemission study of alphaFe2O3. Phys. Rev. B. 66, 085115 (2002). 

J Woicik, E Nelson, I Kronik, M Jain, I Chelikowsky, D 

Heskett, L Berman, G Herman. Hybridization and 

bond-orbital components in site-specific x-ray 

photoelectron spectra of rutile tio2. Phys. Rev. Lett.. 

89 (7), 077401 (2002). 

Beamline X24C

W Hunter, M Kowalski, J Rife, R Cruddace. 

Investigation of the properties of an ion-etched plane 

laminar holographic grating. Appl. Optics-OT. 40

(34), 6157-6165 (2001). 

M Kowalski, H Gursky, J Rife, D Yentis, R Cruddace, T 

Barbee, W Goldstein, J Kordas, K Heidemann, et al.. 

Efficiency calibration of the four multilayer-coated 

holographic ion-etched flight gratings for a sounding 

rocket high-resolution spectrometer. UV/EUV and 

Visible Space Instrumentation for Astronomy and 

Solar Physics, Vol 4498, p. 303-314, sponsored by 

SPIE. (2001). 
Activity Report 2002 7 - 24 

J Long, S Chase, M Kabler. Photoelectron Spectroscopy 

of Exciton Dynamics and Interactions in Organic Thin 

Films: C60 and Photopolymerized C60. AVS 48th

International Symposium, Vol 15, sponsored by AVS. 

(2001). 

Beamline X25

M Baniecki, W McGrath, Z Dauter, W Mangel. 

Adenovirus proteinase: crystallization and preliminary 

X-ray diffraction studies to atomic resolution. Acta 

Cryst. D. D58, 1462-1464 (2002). 

D Battle, J Doudna. Specificity of RNA-RNA Helix 

Recognition. Proc Natl Acad Sci USA. 99 (18), 11676-

11681 (2002). 

B Benoff, H Yang, C Lawson, G Parkinson, J Liu, E 

Blatter, Y Ebright, H Berman, R Ebright. Structural 

Basis of Transcription Activation: the CAP-alphaCTDDNA Complex. Science. 297, 1562-1566 (2002). 

L Berman, Z Yin, Q Shen, K Finkelstein, P Doing, G 

Pan. Characterization Of A Diamond Crystal X-Ray 

Phase Retarder. Rev. Sci. Instrum.. 73 (3), 1502-

1504 (2002). 

L Berman, P Siddons, P Montanez, A Lenhard, Z Yin. A 

Cryogenically Cooled Channel-cut Crystal 

Monochromator Using a Helium Refrigerstor and Heat 

Exchanger. Rev. Sci. Instrum.. 73 (3), 1481-1484 

(2002). 

X Bi, R Corpina, J Goldberg. Structure of the Sec23/24-

Sar1 Pre-budding Complex of the COPll Vesicle Coat. 

Nature. 419, 271-277 (2002). 

E Campbell, S Masuda, J Sun, O Muzzin, J Anders 

Olson, S Wang, S Darst. Crystal Structure of the 

Bacillus stearothermophilus Anti- sFactor SpoIIAB 

with the Sporulation s Factor sF.. Cell. 108, 795-807 

(2002). 

E Campbell, O Muzzin, M Chlenov, J Sun, C Olson, O 

Weinman, M Trester-Zedlitz, S Darst. Structure of the 

Bacterial RNA Polymerase Promoter Specificity Sigma 

Subunit. Mol. Cell. 9, 527-539 (2002). 

T Chiu, C Sohn, R Dickerson, R Johnson. Testing 

Water-mediated DNA Recognition by the Hin 

Recombinase. EMBO J.. 21, 801-814 (2002). 

H Cho, D Leahy. Structure of the extracellular region of 

HER3 reveals an interdomain tether. Science. 297, 

1330-3 (2002). 

D Desveaux, J Allard, N Brisson, J Sygusch. A New 

Family of Plant Transcription Factors Displays a Novel 

ssDNA-binding Surface. Nat. Struct. Biol.. 9 (7), 512-

517 (2002). 

S Dhe-Paganon, K Duda, M Iwamoto, Y Chi, S 

Shoelson. Crystal Structure of the HNF4 alpha Ligand 

Domain in Complex with Endogenous Fatty Acid 

Ligand. J. Biol. Chem.. 277, 37973-37976 (2002). 

E DiMasi, H Tostmann. Surface Induced Order in Liquid 

Metal Alloys. Synch. Rad. News. 12, 41 (1999). 

C Drum, S Yan, J Bard, Y Shen, D Lu, S Soelaiman, Z 

Grabarek, A Bohm, W Tang. Structural Basis for the 

activation of anthrax adenylyl cyclase exotoxin by 

calmodulin. Nature. 415, 396-402 (2002). 

R Dutzler, E Campbell, M Cadene, B Chait, R 

MacKinnon. X-ray structure of a ClC chloride channel 

at 3.0 A reveals the molecular basis of anion 

selectivity. Nature. 415, 287-294 (2002). 

S Gabelli, M Bianchet, Y Ohnishi, Y Ichikawa, M 

Bessman, L Amzel. Mechanism of the Escherichia coli 

ADP-Ribose Pyrophosphatase, a Nudix Hydrolase. 

Biochemistry. 41 (30), 9279 - 9285 (2002). 

R Gilboa, D Zharkov, G Golan, A Fernandes, S 

Gerchman, E Matz, J Kycia, A Grollman, G Shoham. 

Structure of formamidopyrimidine-DNA glycosylase 

covalently complexed to DNA.. J. Biol. Chem.. 277, 

19811-6 (2002). 

Y Ha, D Stevens, J Skehel, D Wiley. H5 Avain and H9 

Swine Influenza Virus Haemagglutinin Structures: 

Possible Origin of Influenza Subtypes. EMBO J.. 21, 

865-875 (2002). 

K Hamalainen, S Manninen. Resonant and NonResonant Inelastic X-Ray Scattering. J. Phys.: 

Condens. Matter. 13, 7539 (2001). 

D Ho, G Coburn, Y Kang, B Cullen, M Georgiadis. The 

Crystal Structure and Mutational Analysis of a Novel 

RNA-Binding Domain Found in the Human Tap 

Nuclear mRNA Export Factor. Proc Natl Acad Sci USA. 

99, 1888-1893 (2002). 

H Ishibashi, T Yoo, Y Hor, A Borissov, Y Horibe, P 

Radaelli, S Cheong, V Kiryukhin. X-ray-induced 

Disordering of the Dimerization Pattern and Apparent 

Low-temperature Enhancement of Lattice Symmetry 

in Spinel CuIr2S4. Phys. Rev. B: Condens. Matter. 

66, 144424 (2002). 

Y Jiang, A Lee, J Chen, M Cadene, B Chait, R 

MacKinnon. Crystal structure and mechanism of a 

calcium-gated potassium channel. Nature. 417, 515-

522 (2002). 

Y Jiang, A Lee, J Chen, M Cadene, B Chait, R 

MacKinnon. The open pore conformation of potassium 

channels. Nature. 417, 523-526 (2002). 

Y Jiang, A Pico, M Cadene, B Chait, R MacKinnon. 

Structure of the RCK domain from the E. coli K+ 

channel and demonstration of its presence in the 

human BK channel. Neuron. 29, 593-601 (2001). 

J Kieft, K Zhou, A Grech, R Jubin, J Doudna. Crystal 

Structure of an RNA Tertiary Domain Essential to HCV 

IRES-mediated Translation Initiation. Nat. Struct. 

Biol.. 9 (370-374)(2002). 

H Li, T Ryan, K Chave, P Van Roey. Three-dimensional 

structure of human gamma-glutamyl hydrolase: a 

class I glutamine amidotransferase adapted for a 

complex substrate. J. Biol. Chem.. 277 (27), 24522-

24529 (2002). 

S Liemann, K Chandran, T Baker, M Nibert, S Harrison. 

Structure of the Reovirus Membrane-Penetration 

Protein, u1, in a Complex with it's Protector Protein 

s3. Cell. 108, 283-295 (2002). 

T Lister, Y Chu, W Cullen, H You, R Yonco, J Mitchell, Z 

Nagy. Electrochemical and X-ray scattering study of 

well defined RuO2 single crystal surfaces. J. 

Electroanal. Chem.. 524, 201 (2002). 

M Marino, M Banerjee, R Jonquieres, P Cossart, P 

Ghosh. GW domains of the L. monocytogenes 

invasion protein InlB are SH3-like and mediate 

binding to host ligands. EMBO J.. 21, 5623-5634 

(2002). 

L Mello, B deGroot, S Li, M Jedrzejas. Structure and 

Flexibility of Steptococcus agalactiae Hyaluronate 

Lyase Complex with its Substrate. J. Biol. Chem.. 

277 (39), 36678-36688 (2002). 
7 - 25 Publications

S Montano, M Cote, I Fingerman, M Pierce, A Vershon, 

M Georgiadis. Crystal Structure of the DNA-binding 

Domain from Ndt80, a Transcriptional Activator 

Required for Meiosis in Yeast. Proc Natl Acad Sci USA. 

99 (22), 14041-14046 (2002). 

A Mulichak, H Losey, C Walsh, R Garavito. Structure of 

the UDP-glucosyltransferase GtfB that modifies the 

heptapeptide aglycone in the biosynthesis of 

vancomycin group antibiotics. Structure. 9, 547-557 

(2001). 

K Murakami, S Masuda, E Campbell, O Muzzin, S Darst. 

Structural basis of transcription initiation: An RNA 

polymerase holoenzyme/DNA complex. Science. 296, 

1285-1290 (2002). 

K Murakami, S Masuda, S Darst. Structural basis of 

transcription initiation: T. aquaticus RNA polymerase 

holoenzyme at 4 Å resolution. Science. 296, 1280-

1284 (2002). 

A Prota, D Sage, T Stehle, J Fingeroth. The Crystal 

Structure of Human CD21: Implications for EpsteinBarr Virus and C3d Binding. Proc Natl Acad Sci USA. 

99 (16), 10641-10646 (2002). 

M Renatus, H Stennicke, F Scott, R Liddington, G 

Salvesen. Dimer Formation Drives the Activation of 

the Cell Death Protease Caspase 9. Proc Natl Acad Sci 

USA. 98, 14250-14255 (2002). 

M Sintchak, G Arjara, B Kellogg, J Stubbe, C Drennan. 

The Crystal Structure of Class II Ribonucleotide 

Reductase Reveals How an Allosterically Regulated 

Monomer Mimics a Dimer. Nat. Struct. Biol.. 9 (4), 

293-300 (2002). 

S Soelaiman, K Jakes, N Wu, C Li, M Shoham. Crystal 

Structure of Colicin E3: Implications for Cell Entry 

and Ribosome Inactivation. Mol. Cell. 8, 1053-1062 

(2001). 

E Sundberg, M Sawicki, S Southwood, P Andersen, A 

Sette, R Mariuzza. Minor Structural Changes in 

Mutated Human Melanoma Antigen Correspond to 

Dramatically Enhanced Stimulation of a CD4+ Tumorinfiltrating Lymphocyte Line. J. Mol. Biol.. 319 (2), 

449-461 (2002). 

F Valiyaveetil, Y Zhou, R MacKinnon. lipids in the 

structure, folding, and function of the KcsA K(+) 

channel. Biochemistry. 41 (35), 10771-10777 

(2002). 

L Zhang, J Doudna. Structural insights into group II 

intron catalysis and branch-site selection. Science. 

295, 2084-8 (2002). 

R Zhao, E Collins, R Bourret, R Silversmith. Structure 

and Catalytic Mechanism of the E. Coli Chemotaxis 

Phosphatase CheZ. Nat. Struct. Biol.. 9 (8), 570-575 

(2002). 

D Zharkov, G Golan, R Gilboa, A Fernandes, S 

Gerchman, J Kycia, R Reiger, A Grollman, G Shoham. 

Structural analysis of Escherichia coli endonuclease 

VIII: its covalent reaction intermediate. EMBO J.. 21, 

789-800 (2002). 

Beamline X26A

Y Arai, D Sparks. Residence Time Effects on Arsenate 

Surface Speciation at the Aluminum Oxide-water 

Interface. Soil Sci. 167, 303-314 (2002). 

A Banas, W Kwiatek, W Zajac. Trace element analysis 

of tissue section by means of synchrotron radiation: 

the use of GNUPLOT for SRIXE spectra analysis. J. 

Alloys Compd.. 328, 135-138 (2001). 

W Bassett, A Anderson, R Mayanovic, I Chou. 

Hydrothermal diamond anvil cell for XAFS studies of 

first-row transition elements in aqueous solution up 

to supercritical conditions. Chem. Geol.. 167, 3-10 

(2000). 

A Becker, W Klock, K Friese, P Schreck, H Treutler, B 

Spettel, M Duff, W Eisenacher. Lake Susser See as a 

natural sink for heavy metals from copper mining. J 

Geochem. Explor.. 74 (1-3), 205-217 (2001). 

E Bloodaxe, J Hughes, M Dyar, E Grew, C Guidotti. 

Tourmaline: linking structure and chemistry. Am. 

Mineral.. 84, 922-928 (1999). 

S Bosze, J Rakovan. Surface structure controlled 

sectoral zoning of REE, Sr, and Y in fluorite. Geochim. 

Cosmochim. Acta. 66, 997-1009 (2002). 

J Cole, J Nienstedt, G Spataro, E Rasbury, A Lanzirotti, 

A Celestian, M Nilsson, G Hanson. Phosphor imaging 

as a tool for in situ mapping of ppm levels of uranium 

and thorium in rocks and minerals. Chem. Geol.. 193

(1-2), 127-136 (2002). 

C Dalpe, D Baker. Experimental investigation of large 

ion lithophile element, high field strength element, 

and rare earth element partitioning between calcic 

amphibole and basaltic melt: the effects of pressure 

and oxygen fugacity. Contrib. Mineral Petr.. 140, 

233-250 (2000). 

A Davenport, M Ryan, M Simmonds, P Ernst, R 

Newman, S Sutton. In situ synchrotron x-ray 

microprobe studies of passivation thresholds in Fe-Cr 

alloys. J. Electrochem. Soc.. 148 (6), B217-B221 

(2001). 

J Delaney, M Dyar, S Sutton. Quantifying X-ray 

pleochroism effects in synchrotron micro-XANES 

analysis of elemental oxidation states. Lunar and 

Planetary Science Conference, Vol 32, p. 1936, 

sponsored by Lunar and Planetary Institute. (2001). 

J Delaney, M Dyar. What we should be looking for in 

Martian meteorites? Is evidence of crustal process or 

mantle process more important... and to whom?. 

Unmixing the SNC's, p. 6021, sponsored by Lunar 

and Planetary Institute. (2002). 

J Delaney, M Dyar. Compositional and oxidation state 

zoning in martian pyroxene: Paradox or process 

indicator. Lunar and Planetary Science Conference, 

Vol 33, p. 1659, sponsored by Lunar and Planetary 

Institute. (2002). 

J Delaney, G Mollel, G Ashley, M Dyar, S Sutton. 

Micrometer scale ferric/ferrous zoning quantified by 

synchrotron micro-XANES spectroscopy of pyroxene 

phenocrysts in phonolitic eruptives from PlioPleistocene volcano, Satiman, Tanzania. Eos, 

Transactions of the American Geophysical Union, Fall 

Meeting Suppl., Vol 82, p. V32D-0996, sponsored by 

EOS Trans, AGU. (2001). 

J Delaney, M Dyar. Magmatic magnetite in martian 

meteorite melt inclusions from Chassigny. Meteoritics 

& Planet. Sci.. 36 Suppl, A48 (2001). 

M Duff, J Coughlin, D Hunter. Uranium Co-precipitation 

with Iron Oxide Minerals. Geochim. Cosmochim. Acta. 

66 (20), 3533-3547 (2002). 
Activity Report 2002 7 - 26 

M Dyar, G Rossman, J Delaney, S Sutton, M Newville. 

Interpretations of Fe-XANES pre-edge spectra: 

predoctions based on Co and Fe optical spectra. 

Lunar and Planetary Science Conference, Vol 32, p. 

1816, sponsored by Lunar and Planetary Institute. 

(2001). 

M Dyar, J Delaney, C Tegner. Ferric iron in feldspar as 

an indicator of evolution of planetary oxygen 

fugacity. Lunar and Planetary Science Conference, 

Vol 32, p. 1065, sponsored by Lunar and Planetary 

Institute. (2001). 

M Dyar, J Delaney, S Sutton. Fe XANES spectra of ironrich micas. Eur. J. Mineral.. 13 (6), 1079-1098 

(2001). 

M Dyar, E Lowe, C Guidotti, J Delaney. Fe3+ and Fe2+ 

partitioning among silicates in metapelites: A 

synchrotron micro-XANES study. Am. Mineral.. 87, 

514-522 (2002). 

M Dyar. Mossbauer and optical spectra of micas. 

Advances in Micas, p. 313-349, Mineralogical Society 

of America, Washington. (2002). 

M Dyar, M Gunter, J Delaney, A Lanzirotti, S Sutton. 

Use of the spindle stage for orientation of single 

crystals for microXAS: Isotropy and anisotropy in FeXANES spectra. Am. Mineral.. 87, 1500-1504 (2002). 

E Elzinga, R Reeder. X-ray absorption spectroscopy 

study of Cu2+ and Zn2+ adsorption complexes at the 

calcite surface: Implications for site-specific metal 

incorporation preferences during calcite crystal 

growth. Geochim. Cosmochim. Acta. 66 (22), 3943-

3954 (2002). 

J Flinn, D Hunter, A Lanzirotti, B Jones. Effects of 

Enhanced in Drinking Water on Brain and Memory. 

Biogeomon, 4th International Conference, Vol 1, p. 

47, sponsored by Villasnova University, Czech 

Geological Survey. (2002). 

J Fredricon, J Zachara, D Kennedy, C Liu, M Duff, D 

Hunter, A Dohnalkova. Influence of Mn oxides on the 

reduction of U(VI) by the metal-reducing bacterium 

Shewanella putrefaciens. Geochim. Cosmochim. Acta. 

66 (18), 3247-3262 (2002). 

C Guest, D Schulze, I Thompson, D Huber. Correlating 

Manganese X-Ray Absorption Near-Edge Structure 

Spectra with Extractable Soil Manganese. Soil Sci. 

Soc. Am. J.. 66, 1172-1181 (2002). 

M Gunter, M Dyar, J Delaney, S Sutton, A Lanzirotti. 

Effects of preferred orientation on microscale XANES 

measurements of Fe3+/total Fe in biopyriboles. Lunar 

and Planetary Science Conference, Vol 33, p. 1654, 

sponsored by Lunar and Planetary Institute. (2002). 

D Hunter, W Gates, P Bertsch, K Kemner. Degradation 

of tetraphenylboron at hydrated smectite surfaces 

studied by time resolved IR and X-ray absorption. 

Mineral Water Interfacial Reactions: Kinetics and 

Mechanisms, p. 282-300, American Chemical Society, 

(1999). 

W Kwiatek, M Galka, A Hanson, C Paluszkiewicz, T 

Cichocki. XANES as a tool for iron oxidation state 

determination in tissues. J. Alloys Compd.. 328, 276-

282 (2001). 

E Lowe. Distribution coefficients for ferric and ferrous 

iron in metapelites from western Maine. B.A. Thesis. 

Mount Holyoke College, South Hadley. (2000). 

R Martin, T Sham, G Wong Won, K Jones, H Feng. 

Synchrotron X-ray Fluorescence and Secondary Ion 

Mass Spectroscopy In Tree Ring Microanalysis: 

Applications to Dendroanalysis. X-Ray Spectrom.. 30, 

338-341 (2001). 

A Mottana, A Marcelli, G Cibin, M Dyar. X-ray 

absorption spectroscopy of micas. Advances in Micas, 

p. 371-412, Mineralogical Society of America, 

Washington. (2002). 

S Naftel, R Martin, K Jones, H Feng, M Savard, C Begin. 

Synchrotron Radiation Analysis of a Smelter 

Impacted Tree Ring Sample. Can. J. Anal. Sci. 

Spectros.. 46 (4), 118-122 (2001). 

J Rakovan. The role of crystal surface structure during 

growth: Trace element incorporation and epitaxy. 

Ph.D. Thesis. SUNY Stony Brook, Stony Brook. 

(1996). 

K Righter, M Dyar, J Delaney, T Vennemann, R Hervig. 

Distribution of OH, O, CL, and F in biotite from 

volcanic rocks and correlations with octahedral 

cations. Am. Mineral.. 87 (1), 142-153 (2002). 

C Tegner, J Delaney, M Dyar. Ferric/ferrous iron in 

plagioclase of the Skaergaard intrusion. EOS. 82

(47), V32E-1037 (2001). 

J Therkelsen, M Dyar, J Delaney, J Johnson, F Horz. 

Effects of shock on ferric iron and major elements in 

plagioclase, pyroxene, and olivine: First 

reconnaisance. Lunar and Planetary Science 

Conference, Vol 33, p. 1696, sponsored by Lunar and 

Planetary Institute. (2002). 

J Therkelsen. Shock-induced changes in redox state of 

experimentally shocked plagioclase, pyroxene, and 

olivine. B.A. Thesis. Amherst College, Amherst. 

(2000). 

J Therkelsen, M Dyar, J Delaney. Geologic and 

Temporal Constraints on the Martian Dichotomy using 

Outflow Channels. Lunar and Planetary Science 

Conference, Vol 33, p. 1696, sponsored by Lunar and 

Planetary Institute. (2002). 

D Vaniman, S Chipera, D Bish, M Duff, D Hunter. 

Crystal chemistry of clay-Mn oxide associations in 

soils, fractures, and matrix of the Bandelier Tuff, 

Pajarito Mesa, New Mexico. Geochim. Cosmochim. 

Acta. 66 (8), 1349-1374 (2002). 

D Vanko, M Bonnin-Mosbah, P Philippot, E Rodder, S 

Sutton. Fluid inclusion in quartz from oceanic 

hydrothermal specimens and the Bingham, Utah, 

porphyry-Cu deposit: a study with PIXE and SXRF. 

Chem. Geol.. 173 (1-3), 227-238 (2001). 

M Vasquez, G Halada, C Clayton. The application of 

synchrotron-based spectroscopic techniques to the 

study of chromate conversion coatings. Electrochim. 

Acta. 47, 3105-3115 (2002). 

D Xirouchakis, D Draper, C Schwandt, A Lanzirotti. 

Crystallization conditions of Los Angeles, a basaltic 

Martian meteorite. Geochim. Cosmochim. Acta. 66, 

181-194 (2002). 

Beamline X26C

E Enemark, A Stenlund, L Joshua-Tor. Crystal 

structures of two intermediates in the assembly of 

the papillomavirus replication initiation complex. 

EMBO J.. 21 (6), 1487-1496 (2002). 
7 - 27 Publications

R Gilboa, D Zharkov, G Golan, A Fernandes, S 

Gerchman, E Matz, J Kycia, A Grollman, G Shoham. 

Structure of formamidopyrimidine-DNA glycosylase 

covalently complexed to DNA.. J. Biol. Chem.. 277, 

19811-6 (2002). 

B Hall, D Bar-Sagi, N Nassar. The Structural basis for 

the transition from Ras.GTP to Ras.GDP. Proc Natl 

Acad Sci USA. 99 (19), 12138 (2002). 

I Hayashi, K Vuori, R Liddington. The focal adhesion 

targeting (FAT) domain of focal adhesion kinase is a 

four-helix bundle that binds paxillin. Nat. Struct. 

Biol.. 9 (2), 101-109 (2002). 

T Messick, N Chmiel, M Golinelli, M Langer, L JoshuaTor, S David. Noncysteinyl coordination to the [4Fe4S]2+ Cluster of the DNA Repair Adenine Glycosylase 

MutY introduced via Site-Directed Mutagenesis. 

Structural Characterization of an Unusual Histidinyl 

Coordinated Cluster. Biochemistry. 41 (12), 3931-

3942 (2002). 

J Min, X Zhang, X Cheng, S Grewal, R Xu. Structure of 

the SET Domain Histone Lysine Methyltransferase 

Clr4. Nat. Struct. Biol.. 9 (11), 828 (2002). 

J Truglio, K Theis, S Leimkuhler, R Rappa, K 

Rajagopalan, C Kisker. Crystal Structures of the 

Active and Alloxanthine-Inhibited Forms of Xanthine 

Dehydrogenase from Rhodobacter capsulatus. 

Structure. 10 (1), 115-125 (2002). 

D van Aalten, W Crielaard, K Hellingwerf, L Joshua-Tor. 

Crystal structure of the photoactive yellow protein 

reconstituted with caffeic acid at 1.16 Å resolution. 

Acta Cryst. D. 58 (4), 585-590 (2002). 

D van Aalten, A Haker, J Hendriks, K Hellingwerf, L 

Joshua-Tor, W Crielaard. Engineering photocycle 

dynamics: crystal structures and kinetics of three 

photoactive yellow protein hinge-binding mutants. J. 

Biol. Chem.. 277 (8), 6463-6468 (2002). 

Z Zhang, M Hayashi, O Merkel, B Stillman, R Xu. 

Structure and Function of the BAH-containing Domain 

of Orc1p in Epigenetic Silencing. EMBO J.. 21 (17), 

4600-4611 (2002). 

D Zharkov, G Golan, R Gilboa, A Fernandes, S 

Gerchman, J Kycia, R Reiger, A Grollman, G Shoham. 

Structural analysis of Escherichia coli endonuclease 

VIII: its covalent reaction intermediate. EMBO J.. 21, 

789-800 (2002). 

Beamline X27C

B Chu. Benjamin Chu. Macromolecules. 35 (3), 585-

586 (2002). 

M Gelfer, A Waddon, K Schmidt-Rohr, R Gale, L 

Kleiner, R Bergren. Annealing_induced Increase of 

Permeability and Amophous-Phase Mobility in 

Ethylene-Vinylacetate Copolymer. J. Polym. Sci., Part 

B: Polym. Phys.. 39, 2774-2779 (2002). 

F Grohn, X Gu, G Nisato, H Grull, B Bauer, E Amis. 

Organization of Hybrid Dendrimer-Inorganic 

Nanoparticles on Amphiphilic Surfaces. 

Macromolecules. 35, 4852 (2002). 

F Grohn, B Bauer, E Amis. Quantum Dots in Dendrimer 

Templates - Small Angle X-ray Scattering Allows to 

Characterize New Nanoparticles with Promising 

Properties. NSLS, Brookhaven. Prepared for DOE. 

(2001). 

F Grohn, B Bauer, E Amis. Hydrophobically Modified 

Dendrimers as Inverse Micelles: Formation of 

Cylindrical Multi-Dendrimer Nanostructures. 

Macromolecules. 34, 6701 (2001). 

F Grohn, G Kim, B Bauer, E Amis. Nanoparticle 

Formation within Dendrimer-Containing Polymer 

Networks: Route to new Organic-Inorganic Hybrid 

Materials. Macromolecules. 34, 2179 (2001). 

J Gu, S Xu, L Yu. A Model of Cross-Bridge Attachment 

to Actin in the A.M.ATP State Based on X-Ray 

diffraction from Permeabilized Rabbit Psoas muscle. 

Biophys. J.. 82, 2123-2133 (2002). 

B Hsiao, F Yeh, L Liu. Nanotailored Crystalline 

Morphology in Hexagonally Perforated Layers of a 

Self-Assembled PS-b-PEO Diblock Copolymer. 

Macromolecules. 35 (9), 3553-3562 (2002). 

G Kumaraswamy, J Kornfield, F Yeh, B Hsiao. ShearEnhanced Crystallization in Isotactic Polypropylene. 

3. Evidence for a Kinetic Pathway to Nucleation. 

Macromolecules. 35 (5), 1762-1769 (2002). 

Z Liu, S Chattopadhyay, M Shaw. The Structurization 

and Rheology of Diblock Copolymer/Hydrocarbon 

Solutions. The Society of Rheology 74th Annual 

Meeting , Vol 74, p. 95, sponsored by The Society of 

Rheology. (2002). 

R McKiernan, A Heintz, S Hsu, E Atkins, J Penelle, S 

Gido. Influence of Hydrogen Bonding on the 

Crystallization Behavior of Semicrystalline 

Polyurethanes. Macromolecules. 35, 6970-6974 

(2002). 

C Park, J McAlvin, C Fraser, E Thomas. Iron Cluster and 

Microstructure Formation in Metal-Centered Star 

Block Copolymers: Amphiphilic Iron Tris(bipyridine)-

Centered Polyoxazolines. Chem. Mater.. 14 (3), 

1225-1230 (2002). 

S Ran, X Zong, D Fang, B Hsiao, B Chu, P Cunniff, R 

Phillips. Studies of the mesophase development in 

polymeric fibers during deformation by synchrotron 

SAXS/WAXD. J. Mater. Sci.. 36, 3071-3077 (2001). 

S Ran, C Burger, D Fang, X Zong, S Cruz, B Chu, B 

Hsiao, R Bubeck, K Yabuki, et al. In-Situ Synchrotron 

WAXD/SAXS Studies of Structural Development 

during PBO/PPA Solution Spinning. Macromolecules. 

35 (2), 433-439 (2002). 

F Schipper, G Fouldas, S Pispas, N Hadjichristidis, T 

Pakula. The Phase State of Poly(butadiene-b-tertbutyl methacrylate) and Poly(ethylene-b-tert-butyl 

methacrylate) Diblock Copolymers. Macromolecules. 

35, 8860-8868 (2002). 

S Toki, I Sics, S Ran, L Liu, B Hsiao, S MurakamiI, K 

Senoo, S Kohjiya. New Insights into Structural 

Development in Natural Rubber During Uniaxial 

Deforemation in situ Synchrotron X-ray Diffraction. 

Macromolecules. 35 (17), 6578 (2002). 

S Xu, J Gu, G Melvin, L Yu. Structural Characterization 

of Weakly Attached Cross-Bridges in the A.M.ATP 

State in Permeabilized Rabbit psoas Muscle. Biophys. 

J.. 82, 2111-2122 (2002). 

L Zhu, P Huang, W Chen, Q Ge, R Quirk, S Cheng, E 

Thomas, B Lotz, B Hsiao, et al. Nanotailored 

Crystalline Morphology in Hexagonally Perforated 

Layers of a Self-Assembled PS-b-PEO Diblock 

Copolymer. Macromolecules. 35, 3553-3562 (2002). 
Activity Report 2002 7 - 28 

Y Zhu, R Weidisch, S Gido, G Velis, N Hadjichristidis. 

Morphologies and Mechanical Properties of a Series of 

Block-Double-Graft Copolymers and Terpolymers. 

Macromolecules. 35, 5903-5909 (2002). 

L Zhu, B Mimnaugh, Q Ge, R Quirk, S Cheng, E 

Thomas, B Lotz, B Hsiao, F Yeh, L Liu. Hard and soft 

confinement effects on polymer crystallization in 

microphase separated cylinder-forming PEO-b-PS/PS 

blends. Polymer. 42 (21), 9121 (2001). 

Beamline X28C

M Chance. Unfolding of Apomyoglobin Examined by 

Synchrotron Footprinting. Biochem. Biophys. Res. 

Commun.. 287, 614-621 (2001). 

G Dhavan, D Crothers, M Chance, M Brenowitz. 

Concerted Binding and Bending of DNA by Eschericia 

Coli Integration Host Factor . J. Mol. Biol.. 315, 

1027-1037 (2002). 

S Goldsmith, J Guan, S Almo, M Chance. Synchrotron 

Protein Footprinting: A Technique to Investigate 

Protein-Protein Interactions. J. Biomol. Struct. Dyn.. 

19, 405-419 (2001). 

J Guan, S Vorobiev, S Almo, M Chance. Mapping the GActin Binding Surface of Cofilin Using Synchrotron 

Protein Footprinting. Biochemistry. 41 (18), 5765-

5775 (2002). 

S Heilman-Miller, J Pan, D Thirumalai, S Woodson. Role 

of Counterion Condensation in Folding of the 

Tetrahymena Ribozyme II Counterion-Dependence of 

Folding Kinetics. J. Mol. Biol.. 309, 57-68 (2001). 

J Kiselar, S Maleknia, M Sullivan, K Downard, M 

Chance. Hydroxyl Radical Probe of Protein Surfaces 

Using Synchrotron X-Ray Radiolysis and Mass 

Spectrometry. Int. J. Radiat. Biol.. 78, 101-114 

(2002). 

S Maleknia, C Ralston, M Brenowitz, K Downard, M 

Chance. Determination of Macromolecular Folding 

and Structure by Synchrotron X-Ray Radiolysis 

Techniques. Anal. Biochem.. 289, 103-115 (2001). 

D Thirumalai, N Lee, S Woodson, D Klimov. Early 

Events in RNA Folding. Annu. Rev. Phys. Chem.. 52, 

751-762 (2001). 

T Uchida, Q He, C Ralston, M Brenowitz, M Chance. 

Linkage of Monovalent and Divalent Ion Binding in 

the Folding of the P4-P6 Domain of the Tetrahymena 

Thermophila Ribozyme. Biochemistry. 41, 5799-5806 

(2002). 

S Woodson, M Deras, M Brenowitz. Time-Resolved 

Hydroxyl Radical Footprinting of RNA with X-Rays. 

Current Protocols in Nucleic Acid Chemistry , p. 

11.6.1-11.6.23, John Wiley Sons, New York. 
7 - 1 Publications

NSLS Staff 

J Ablett, C Kao, A Lunt. The Design and Performance 

Of An X-Ray Micro-Focusing System Using 

Differentially Deposited Elliptical Mirrors At The 

National Synchrotron Light Source. Rev. Sci. 

Instrum.. 73 (10), 3464-3468 (2002). 

I Baek, S Hulbert, E Vescovo. Performance of a 

quadruple reflector circular polarizer in VUV region 

for angle-and spin-resolved photoemission 

spectroscopy. Scripta Mater.. 73 (3), 1496-1498 

(2002). 

I Ben-Zvi, M Babzien, E Blum, W Casey, X Chang, W 

Graves, J Hastings, S Hulbert, E Johnson, et al.. 

Photoinjected Energy Recovery Linac Upgrade for the 

NSLS. 2001 IEEE Particle Accelerator Conference, 

June 2001, (Paper WOAB005), sponsored by IEEE. 

(2001). 

I Ben-Zvi, L Ahrens, M Brennan, M Harrison, J J. 

Kewisch, W MacKay, S Peggs, T Roser, T Satogata, 

et al.. Electron Cooling For RHIC. 2001 IEEE Particle 

Accelerator Conference, June 2001, (Paper 

MOPA011), sponsored by IEEE. (2001). 

L Berman, P Siddons, P Montanez, A Lenhard, Z Yin. A 

Cryogenically Cooled Channel-cut Crystal 

Monochromator Using a Helium Refrigerstor and 

Heat Exchanger. Rev. Sci. Instrum.. 73 (3), 1481-

1484 (2002). 

L Berman, Z Yin, Q Shen, K Finkelstein, P Doing, G 

Pan. Characterization Of A Diamond Crystal X-Ray 

Phase Retarder. Rev. Sci. Instrum.. 73 (3), 1502-

1504 (2002). 

P Bolton, J Clendenin, D Dowell, M Ferrario, A Fisher, S 

Gierman, R Kirby, P Krejcik, C Limborg, et al.. 

Photoinjector design for the LCLs. Nucl. Instrum. 

Meth. A. 483, 296-300 (2002). 

M Cole, H Bluem, J Rathke, T Schulteiss, I Ben-Zvi, T 

Srinivasan-Rao. Progress Toward An All Niobium 

Superconducting RF Photocathode Electron Gun. 

2001 IEEE Particle Accelerator Conference, June 

2001, (Paper WOAB005), sponsored by IEEE. 

(2001). 

M Corwin. NSLS 2001 Activity Report (National 

Synchrotron Light Source Activity Report 2001). 

Government Printing Office, Upton. (2002). 

M Croft, I Zakharchenko, Z Zhong, Y Gulak, J 

Hastings, J Hu, R Holtz, M DaSilva, T Tsakalakos. 

Strain Field and Scattered Intensity Profiling with 

Energy Dispersive X-Ray Scattering. J. Appl. Phys.. 

92, 578-586 (2002). 

E DiMasi. The Search for Liquid Fivefold Symmetry. 

Phys. World. 14, 20 (2001). 

M Farmer, L Boatner, B Chakoumakos, C Rawn, J 

Richardson, S Khalid. Polymorphism and a phase 

transition in K3Yb(PO4)2. International Union of 

Crystallography, Geneva, Switzerland, Vol XIX, p. x, 

sponsored by International Union of Crystallography. 

(2002). 

P Frigola, A Murokh, P Musumeci, C Pellegrini, S 

Reiche, J Rosenzweig, A Tremaine, M Babzien, I BenZvi, et al.. Initial Gain Measurements of a 800nm 

SASE FEL, VISA. The 22nd International Free 

Electron Laser Conference and 7th FEL Users 

Workshop, August 13-18, 2000, sponsored by Free 

Electron Laser Conference 2000. 

W Graves, G Carr, L DiMauro, A Doyuran, R Heese, E 

Johnson, C Neuman, G Rakowsky, J Rose, et al.. 

Ultrashort Electron Bunch Length Measurements at 

DUVFEL. 2001 IEEE Particle Accelerator Conference, 

June 2001, (Paper WPAH058), sponsored by IEEE. 

(2001). 

W Graves, L DiMauro, R Heese, E Johnson, J Rose, J 

Rudati, T Shaftan, B Sheehy, L Yu, et al.. DUVFEL 

Photoinjector Dynamics: Measurement and 

Simulation. 2001 IEEE Particle Accelerator 

Conference, June 2001, (Paper WPAH060), 

sponsored by IEEE. (2001). 

W Graves, G Carr, L DiMauro, A Doyuran, R Heese, E 

Johnson, S Krinsky, C Neuman, G Rakowsky, et al.. 

Measured Properties Of The DUVFEL High Brightness, 

Ultrashort Electron Beam. 2001 IEEE Particle 

Accelerator Conference, June 2001, (Paper 

RPAH008), sponsored by IEEE. (2001). 

Y Hasegawa, Y Ueji, K Okitsu, J Ablett, D Siddons, Y 

Amemiya. Transmission-type X-ray linear polarizer 

with perfect crystals. J. Synch. Rad.. 5 (3), 738-740 

(1998). 

S Heifets, G Stupakov, S Krinsky. CSR Instability in a 

Bunch Compressor. Phys. Rev. ST AB. 5, 064401 

(2002). 

S Heifets, G Stupakov, S Krinsky. Coherent 

Synchrotron Radiation Instability in a Bunch 

Compressor. Phys. Rev. ST AB. 5, 064401 (2002). 

S Heifets, S Krinsky, G Stupakov. Fundamentals of 

Hard X-ray Synchrotron Radiation Sources. ThirdGeneration Hard X-ray Synchrotron Radiation 

Sources: Source, Properties, Optics and 

Experimental Techniques, p. 40, John Wiley & Sons, 

Inc., (2002). 

J Hu, W Casey, D Harder, S Pjerov, G Rakowsky, J 

Skaritka. The Mechanical and Shielding Design of a 

Portable Spectrometer and Beam Dump Assembly at 

BNL's Accelerator Test Facility. 2nd International 

Workshop on Mechanical Engineering Design of 

Synchrotron Radiation Equipment and 

Instrumentation (MEDSI02), Vol 1, p. 8, sponsored 

by Advance Photon Source. (2002). 

S Kashiwagi, M Washio, X Wang, I Ben-Zvi, R Malone, 

V Yakimenko. Photo-Electron Beam Longitudinal 

Phase Space Tomography Studies at the ATF. 20th 

International Linac Conference, Vol 1, p. 149, 

(2000). 

W Kimura, L Campbell, C Dilley, S Gottschalk, D 

Quimby, M Babzien, I Ben-Zvi, J Gallardo, K Kusche, 

et al.. First Demonstration of Staged Laser 

Acceleration. Proceedings of the 2001 Particle 

Accelerator Conference, p. 103-107, sponsored by 

PAC 2001. (2001). 

S Kramer. Direct Observation of Beam Impedance 

Above Cut-off. Phys. Rev. ST AB. 5, 112001-1 

(2002). 

X Li, G Wu, Y Abramov, A Volkov, P Coppens. 

Application of charge density methods to a protein 

model compound: calculation of coulombic 

intermolecular interaction energies from the 

experimental charge density. Proc Natl Acad Sci USA. 

99 (19), 12132-12137 (2002). 
Activity Report 2002 7 - 2 

R Malone, I Ben-Zvi, X Wang, V Yakimenko. BNL 

Accelerator Test Facility Control System Upgrade. 

2001 IEEE Particle Accelerator Conference, June 

2001, (Paper MPPH005), p. 776-778, sponsored by 

IEEE. (2001). 

T Mentes, C Sanchez-Hanke, C Kao. Reconstruction of 

Magnetization Density in 2-Dimensional Samples 

From Soft X-ray Speckle Patterns Using MultipleWavelength Anomalous Diffraction Method. J. Synch. 

Rad.. 9, 90-95 (2002). 

A Murokh, P Frigola, C Pellegrini, J Rosenzweig, A 

Tremaine, E Johnson, X Wang, V Yakimenko, L 

Klaisner, et al.. Intra-undulator Measurements at 

VISA FEL. 2000 International FEL, sponsored by Free 

Electron Laser Conference 2000. (2000). 

A Murokh, J Rosenzweig, I Ben-Zvi, X Wang, V 

Yakimenko. Limitations On Measuring A Transverse 

Profile Of Ultra-Dense Electron Beams With 

Scintillators. 2001 IEEE Particle Accelerator 

Conference, June 2001, (TPAH049), sponsored by 

IEEE. (2001). 

J Murphy, I Ben-Zvi, N Towne, J Wang, X Wang, J Wu, 

V Yakimenko. Beam Dynamics for a Photoinjected 

Energy Recovery Linac at the NSLS. 2001 IEEE 

Particle Accelerator Conference, June 2001, 

(WOPB012), sponsored by IEEE. (2001). 

S Peggs, I Ben-Zvi, J Kewisch, J Murphy. Accelerator 

Physics Issues for Future Electron-Ion Colliders. 

Proceedings of the 2001 IEEE Particle Accelerator 

Conference, p. 37-41, sponsored by IEEE. (2001). 

B Podobedov, G Carr, S Kramer, J Murphy. 

Longitudinal Density Modulation Of Unstable Bunches 

Emitting Coherent IR. 2001 IEEE Particle Accelerator 

Conference, June 2001, (Paper TPPH109), sponsored 

by IEEE. (2001). 

B Podobedov, B Kushner, S Ramamoorthy, Y Tang, E 

Zitvogel. Fast Digital Orbit Feedback Systems at 

NSLS. 2001 IEEE Particle Accelerator Conference, 

June 2001, (Paper WOPA005), sponsored by IEEE. 

(2001). 

Q Qian, T Tyson, C Kao, M Croft, A Yu. Ignatov. Local 

magnetic ordering in La1_xCaMn03 determined by 

spin-polarized x-ray absorption spectroscopy. Appl. 

Phys. Lett.. 80 (17), 3141-3143 (2002). 

G Rakowsky, D Lynch, E Blum, S Krinsky. NSLS InVacuum Undulators and Mini-Beta Straights. 2001 

IEEE Particle Accelerator Conference, June 2001, 

(Paper WPPH003), sponsored by IEEE. (2001). 

G Rakowsky. Enhancement of NSLS Sextupoles Using 

Permanent Magnets. 2001 IEEE Particle Accelerator 

Conference, June 2001, (Paper RPPH012), sponsored 

by IEEE. (2001). 

J Rose, W Graves, R Heese, E Johnson, S Krinsky, B 

Sheehy. Modeling and Measurements Of The DUVFEL 

Photoinjector Cavity RF Properties. 2001 IEEE 

Particle Accelerator Conference, June 2001, (Paper 

WPAH057), sponsored by IEEE. (2001). 

J Rose. Conceptual Design Of A Capture RF System For 

MUON Colliders. 2001 IEEE Particle Accelerator 

Conference, June 2001, (Paper MPPH032), sponsored 

by IEEE. (2001). 

J Rose, J Brennan, A Campbell, S Kwiatkowski, W Pirkl, 

A Ratti. RHIC 28 MHZ Accelerating Cavity System. 

2001 IEEE Particle Accelerator Conference, June 

2001, (Paper MPPH031), sponsored by IEEE. (2001). 

T Shaftan, M Babzien, I Ben-Zvi, S Biedron, L 

DeMauro, A Doyuran, J Galayda, E Gluskin, W 

Graves, etal. High-Gain Harmonic Generation FreeElectron Laser at Saturation. 2001 IEEE Particle 

Accelerator Conference, June 2001, (Paper 

TOPA009), p. 63, sponsored by IEEE. (2001). 

J Tetenbaum, L Miller. A new spectroscopic approach 

to examining the role of disulfide bonds in the 

Structure and Unfolding of Soybean Trypsin 

Inhibitor. Biochemistry. 40, 12215-19 (2001). 

A Tremaine, P Frigola, A Murokh, C Pellegrini, S 

Reiche, J Rosenzweig, M Babzien, I Ben-Zvi, E 

Johnson, et al.. Characterization of an 800 nm SASE 

FEL at saturation. Nucl. Instrum. Meth. A. 483, 24-

28 (2002). 

A Tremaine, X Wang, A Murokh, C Pellegrini, M 

Babzien, I Ben-Zvi, M Cornacchia, H Nuhn, R Malone, 

S Reiche. Experimental Characterization of Nonlinear 

Harmonic Radiation from a Visable Self-Amplified 

Spontaneous Emission Free-Electron Laser at 

Saturation. Phys. Rev. Lett.. 88 (20), 204801(4) 

(2002). 

A Tremaine, X Wang, M Babzien, I Ben-Zvi, M 

Cornacchia, A Murokh, H Nuhn, R Malone, C 

Pellegrini, et al.. Fundamental and Harmonic 

Microbunching Measurements in a High-Gain SelfAmplified Spontaneous Emission Free-Electron Laser. 

Phys. Rev. E. 66, 036503 (2002). 

A Tremaine, X Wang, A Murokh, C Pellegrini, M 

Babzien, I Ben-Zvi, M Cornacchia, H Nuhn, R Malone, 

et al.. Saturation Measurements of a Visible SASE 

FEL. 2001 IEEE Particle Accelerator Conference, June 

2001, (Paper WPPH122), sponsored by IEEE. (2001). 

J Wu, L Yu. High Gain Harmonic Generation X-ray Free 

Electron Laser. 2001 IEEE Particle Accelerator 

Conference, June 2001, (Paper WPPH107), p. 2716, 

sponsored by IEEE. (2001). 

J Wu, L Yu. High Gain Harmonic Generation UV to DUV 

Electron Lasers at the NSLS. 2001 IEEE Particle 

Accelerator Conference, June 2001, (Paper 

WPPH108), p. 2719, sponsored by IEEE. (2001). 

J Wu, J Murphy, V Yakimenko, I Ben-Zvi, W Graves, E 

Johnson, S Krinsky, T Shaftan, L Yu. Coherent 

Synchrotron Radiation Analysis for the Photoinjected 

Energy Recovery Linac and UVFEL Projects At The 

NSLS. 2001 IEEE Particle Accelerator Conference, 

June 2001, (Paper RPAH012), p. 2866, sponsored by 

IEEE. (2001). 

J Wu, L Yu. Eigenmodes and Modes Competition in 

High Gain Free-electron Laser Including Alternatinggradient Focusing. Nucl. Instrum. Meth. A. 475, 79-

85 (2001). 

V Yakimenko, I Ben-Zvi, J Murphy, S Pjerov, J Wu. 

Optics for a Photoinjected Energy Recovery Linac at 

the NSLS. 2001 IEEE Particle Accelerator Conference, 

June 2001, (Paper RPPH051), sponsored by IEEE. 

(2001). 

L Yang, H Huang. Observation of a Membrane Fusion 

Intermediate Structure. Science. 297 (5588), 1877-

1879 (2002). 

L Yu, L DiMauro, A Doyuran, W Graves, E Johnson, S 

Krinsky, S Mikhailov, G Rakowsky, J Skaritka, et al.. 

The DUV-FEL Development Program. 2001 IEEE 

Particle Accelerator Conference, June 2001, (Paper 

WPPH329), sponsored by IEEE. (2001). 
7 - 3 Publications

Y Zhang, S Ehrlich, R Colella, M Kopecky, M Widom. Xray Diffuse Scattering in Icosahedral Quasicrystal AlPd-Mn. Phys. Rev. B. 66, 104202 (2002). 

F Zhou, J Wu, M Babzien, I Ben-Zvi, R Malone, J 

Murphy, X Wang, M Woodle, V Yakimenko. Surface 

Roughness Wakefield Measurement At Brookhaven 

Accelerator Test Facility. Phys. Rev. Lett.. 89, 

174801 (2002). 

F Zhou, I Ben-Zvi, X Wang. Beam Dynamics 

Stimulations For A DC Gun Based Injector For PERL. 

2001 IEEE Particle Accelerator Conference, June 

2001, (Paper WPAH075), p. 2266-2268, sponsored 

by IEEE. (2001).