How to use Solid-State NMR Spectral Database (SSNMR_SD)
1. Home page
2. Search page
3. Display page of search results
4. Display page of spectral data
4-1. NMR parameters
4-2. Chemical shift references
4-3. NMR spectra
4-4. Pulse programs

1. Home page
SSNMR_SD consists of a home page, a search page, a display page of search results and display
pages of spectral data. Although you can access SSNMR_SD freely, we ask you to agree thedisclaimer each time when you use SSNMR_SD. When you click “I agree the disclaimer and usethis database.” button at the bottom of the home page, you will move on to the search page which isan entrance of SSNMR_SD.
2. Search page
Users can search spectral data by using a substance name, an element and a nucleus (or a spin)
as search items. Users do not need to input all the search items.
Click the “Search” button after inputting search items. Clicking the "Clear" button clears all
the input values. Users can choose the number of hit results displayed per page by setting the pull
down menu at the right side of the “Clear” button.
(a) Substance name
Users can use English and Japanese names. The wild card character (*) can be used.
(b) Element
Input an element. Use a blank or a comma (,) when you input more than one element.
When you input more than one element, substances containing all the input elements or none of
the input elements are searched.
You can input the number of carbons contained. The lower limit and the upper limit arespecified.
(c) Nucleus (spin)
Input the nucleus. Use a blank or a comma (,) when you input more than one nucleus.
You can select a nucleus by clicking the nucleus listed in the box. If you want to select more1

than one nucleus from the box, click the nucleus during pressing Ctrl key for Windows and Linux orCommand key for Mac.
3. Display page of search results
Search results are displayed in this page. The page presents information on the substancesand nuclei of spectral data. When you click the nucleus, you move to Display page of spectral data.
4. Display page of spectral data
Display page of spectral data presents the nucleus, information on the substance, titles of NMR
parameters and the titles of NMR spectra. Click one of the titles, and NMR parameters and NMR
spectra are displayed.
The mark "Std" on the titles of NMR parameters and NMR spectra indicates that those are usedin standard NMR measurements.
4-1. NMR parameters
NMR parameters such as chemical shifts (isotropic and anisotropic values), nuclear quadrupole
interaction and so on are displayed. Assignment of each signal is presented when possible.
The mark "Std" indicates that the presented parameters are used in standard NMR
measurements.
Several parameters displayed in NMR parameters are explained below:(1) Assignment: Assignment of each signal is displayed. You can click a “diagram” button if
present to see a structure schematic. When the schematic has numbers on atoms, for example, inthe case of 13C NMR spectra, C(3,5) means that signals of C(3) and C(5) are overlapped, whereas
C(3/5) indicates that the signal is either C(3) or C(5). The mark * in the assignment like C(2*)
means that the assignment is tentative.
(2) Peak position under MAS: Peak positions in MAS NMR spectra are displayed. Quadrupolar
nucleus might show a peak position different from the chemical shift due to the second-order
qudrupole shift. Peak positions are displayed when the chemical shift cannot evaluated or when
we want to display the peak position explicitly,(3) Chemical shift (CS):components

ofa

Parameters of chemical shift interactions are displayed.

chemicalshifttensor

δ11 、 δ22 、 δ33

aredefined

asPrincipal
tosatisfyδ 33 − δ iso ≥ δ 11 − δ iso ≥ δ 22 − δ iso . Isotropic shift δiso, Anisotropy ∆δanis and asymmetry factor ηC areexpressed as follows:13δ iso = (δ 11 + δ 22 + δ 33 )∆δ anis = δ 33 −

δ 11 + δ 222

3= (δ 33 − δ iso )
22

ηC =

δ 22 − δ 11
δ 33 − δ iso( 0 ≤ ηC ≤ 1)

NMR signals are shifted by Knight shift when the substance is metallic. Knight shift has almost
the same NMR property as the chemical shift. Consequently, this database does not differentiate
Knight shift from the chemical shift.
(4) Quadrupole interaction (QI):

Parameters of quadrupole inetarction are displayed for

quadrupolar nucleus (I > 1/2). Principal components of an electric field gradient tensor q 11 ,q 22 , q 33 are defined as to satisfy q33 ≥ q11 ≥ q22 .
relation q11 + q 22 + q 33 = 0 .

The principal components satisfy theQuadrupole coupling constant QCC and asymmetry factor ηQ

are expressed as follows:e 2 Qq33
hq − q11
η Q = 22q33
QCC =( 0 ≤ ηQ ≤ 1)(5) Euler angles between CS and QI:

The axis system is transformed from chemical shiftprincipal axis system (CS-PAS) to quadrupole interaction principal axis system (Q-PAS)with these angles.
(6) Indirect spin coupling (J): Parameters of indirect spin coupling are displayed.
(7) Fraction: Fractions of signals are displayed when two or more than two signals are present.
4-2. Chemical shift references
Chemical shift values in SSNMR_SD are defined with respect to the standard substances inTable 1. In other words, the chemical shifts of the standard substances are defined as 0 ppm.
Table 1. Standard substances for the chemical shift
ChemicalState

NucleusSubstance

1H

tetramethylsilane

Si(CH3)4neat

2H

deuterated water

D2O

neat

3He

helium-3 gas

He

100 kPa

6Li

lithium chloride

LiCl

1.0 M aqueous solution

7Lilithium chloride

LiCl

1.0 M aqueous solution

11B

borontrifluoride-ethylether complex(C2H5)2O⋅BF3

neat

13C

tetramethylsilane

Si(CH3)4

neat

15N

nitromethane

CH3NO2

neat

17O

water

H2O

neat

19F

hexafluorobenzene

C6F6

neat

formula3

23Na

sodium chloride

NaCl

1.0 M aqueous solution

27Al

aluminum nitrate

Al(NO3)3

1.0 M aqueous solution

29Si

tetramethylsilane

Si(CH3)4

neat

31P

phosphoric acidH3PO4

85% aqueous solution

33S

cesium sulfate

Cs2SO4

1.0 M aqueous solution

35Cl

potassium chloride

KClsolid

39K

potassium chloride

KCl

1.0 M aqueous solution

51V

vanadium(V) trichloride oxide

VOCl3

neat

59Co

potassium hexacyanocobaltate(III)K3Co(CN)6

63Cu

cuprous chloride

CuClsolid

65Cu

cuprous chloride

CuCl

solid

77Se

dimethylselenium

Se(CH3)2

neat

79Br

potassium bromide

KBr

solid

87Rb

rubidium chloride

RbCl

1.0 M aqueous solution

93Nb

hexafluoroniobium ion[NbF6]−48% HF aqueous solution

119Sn

tetramethyltin

Sn(CH3)4

neat125Te

dimethyltellurium

Te(CH3)2

neat

127I

potassium iodide

KIsolid

129Xe

xenon gasXe

zero pressure

133Cs

cesium chloride

CsCl1.0 M aqueous solution

195Pt

1H (tetramethylsilane) x 0.214

Si(CH3)4

neat207Pb

tetramethyllead

Pb(CH3)4

neat

saturated aqueoussolution

4-3. NMR spectra
An NMR spectrum is displayed as well as a list of peak positions.

NMR measurement

parameters are displayed when one clicks the "Measurement Parameters" button.

The pulse

program diagram is displayed when one clicks the pulse program name in the Measurement
Parameters window.
The mark "Std" indicates that the presented spectrum is used as a reference in NMR
measurements.
Several parameters displayed in “Measurement Parameters” are explained below:(1) Tmeperature: The temperature indicated by the temperature controller is displayed usually.
“Temperature (calibrated)” is used when the temperature is calibrated. “Temperature (nominal)”
is used when the uncalibrated temperature is displayed as well.
(2) MAS/static: Sample spinning mode is displayed. “MAS” is magic angle spinning, “VAS” isvariable angle spinning, “off-MAS” is off-magic angle spinning and “static” is a static sample. Theangle between the spinning axis and the magnetic field is displayed when the sample is spinning atthe angle other than the magic angle.
4(3) Spinning rate: The spinning rate of the sample is displayed. When the sample is static, thisparameter is not displayed or is 0 kHz.
(4) Probehead: “MAS” is MAS probehead, “BB” is a broadband probehead with a solenoid coil and“HR” is a high resolution probehead for solution.
(5) Observed frequency: The frequency corresponding to the 0-ppm shift position is displayed.
This value is used when the unit is converted between Hz and ppm.
(6) Decoupling frequency: The pulse frequency of the decoupling pulse is displayed.
(7) The pulse widths in Instrument: They are determined for a substance with QCC = 0 in the caseof quadrupolar nucleus.
4-4. Pulse programs
Pulse programs used to acquire the spectral data are listed in Table 2.
Table 2. Pulse programs
Abbreviation

Full nameCPcross polarization

CPTPPM

cross polarization with TPPM decouplingHDsingle pulse with high power decoupling

INEPT-DEC

INEPT with decoupling

INEPT-NON

INEPT without decoupling

QE

solid echo/quadrupole echo

SEspin echo

SPsingle pulse

VACP

cross polarization with variable pulse amplitude for observed spin5