bluuebunny/crossref_metadata_2025 huggingface dataset:
An extension to the principle of congruence
Authors: Williamson AG
Published: September 2010

P.A graphical procedure, analogous to that already used for mixtures of homologues of the general
formula AnB, is described which can be used with mixtures of molecules of the general type, AnBn.
The procedure is tested with enthalpies of mixing of ethers with other ethers and with alkanes.
The mercury(II)-induced aquation of trans-Chloroamminebis(dimethylglyoximato)cobalt(III) complex
Authors: Chan S , Tan S
Published: September 2010

The pseudo first-order rate
constants for the mercury(II)-induced aquation of trans-[Co(Hdmg)2(NH3)Cl] (Hdmg = dimethylglyoximate
ion) have been measured in aqueous and aqueous ethanol solutions (ethanol- water
mole ratio 1 : 5.1) containing various excess amounts of mercury(II)ion at
273.2 K. Association constants of the complex formed with mercury(II) ion and
rate constants for dissociation of the activated complex in both solutions have
been calculated. The kinetic results are discussed in terms of formation of an
activated complex Co-C1-Hg, followed by a simple rate-determining aquation in
which HgCl+ acts as the leaving group.
A tetrameric cobalt(II) cluster of 7-azaindole
Authors: Brookes RW , Martin RL
Published: September 2010

The synthesis and properties
of the tetrameric cobalt(II) complex [Co4O(C7H5N2)6],
where C7H5N2-is the anion of 7-azaindole
(1H-pyrrolo[2,3- b]pyridine), are reported. A tetrameric molecular structure is
indicated by the mass spectrum. The electronic spectrum is consistent with a
tetrahedral environment about each cobalt atom. The compound displays
antiferromagnetic behaviour which conforms to simple Heisenberg theory over the
liquid nitrogen temperature range. The fitted exchange constant J is c. -16 cm-1.
Symmetrization of Bromobis(polyfluorophenyl)thallium(III) compounds with copper powder
Authors: Deacon GB , Vince DG
Published: September 2010

Reaction of bromobis(polyfluorophenyl)thallium(III)
compounds, R2TlBr (R = C6F5, p-HC6F4,
m-HC6F4 or 3,5-H2C6F3)
and (C6F5)2TlOH, with copper powder in boiling
1,4-dioxan (diox) or diethyl ether gave the
corresponding tris(polyfluorophenyl)thallium(III) compounds, which were
isolated as the complexes R3Tl,diox. By contrast, the derivatives R2TlBr
(R = o- HC6F4, 3,6-H2C6F3
or Ph) failed to react, and (C6F5)2TlBr was
decomposed by copper powder in boiling toluene yielding decafluorobiphenyl.
Formation of tris(polyfluorophenyl)thallium(III) compounds is considered to occur
via polyfluorophenylcopper(I) intermediates.
Treatment of (C6F5)2TlBr with pentafluorophenylcopper in dioxan gave (C6F5)3Tl,diox.
The new bromobis-(polyfluorophenyl)thallium(III) compounds, R2TIBr
(R = p-HC6F4, m-HC6F4, o-HC6F4,
3,5-H2C6F3 or 3,6- H2C6F3),
were prepared by reaction of thallic chloride with the appropriate Grignard
reagents.
Reactions of a partially fluorinated diphenylacetylene with some carbonyl complexes of cobalt and rhodium
Authors: Dickson RS , Michel LJ
Published: September 2010

The alkyne C6F4HC~CC6Hs has been isolated from the reaction of phenylethynylcopper(~) with
1,2-diiodotetrafluorobenzene in refluxing pyridine. Spectroscopic properties indicate the alkyne is
phenyl(2,3,4,5-tetrafluoropheny1)ethyne.
The reactions of C6F4HGCC6H5 with (q-C5H,)Co(CO), and (q-C5H5)Rh(CO), have been
compared. With (~-C,H,)CO(CO)~, three isomers of the cyclopentadienone complex
(q-C5H5)Co[C4(C6F4H)Z(C6H5)2CO] were isolated in addition to the cyclobutadiene complex
(q-C5HS)Co[C4(C6F4H)2(C6H5)2] and the substituted benzene C6(C6F4H)3(C6H5)3. The reaction
with (q-C5H5)Rh(C0)2 also gives C6(C6F4H)3(C6H5)3 and three isomers of (q-C,H,)-
Rh[C4(C6F4H)2(C6H5)2CO], but some additional organometallic and organic products are
formed. These include the organorhodium complexes (C5H5)3Rh3(CO)(C6F4HC2C6H5),
(CsH5)3Rh3(C6F4HC2C&) and (C5H5)2Rhz(C6F4HC2C6Hs)2, and an organic compound of
formula (C6F4HC2C6H5)4.
Treatment of CO~(CO)~ with C6F4HC~CC6H5 has given the'p-alkyne complex CO~(CO)~(C~F~H-
C2C6H5). Thermal degradation at 180-190" of this complex yields a range of organic products
including two isomers of the cyclopentadienone compound C4(C6F4H)2(C6H&C0, the
substituted benzene C6(C6F4H)3(C6H5)3, and an oligomer (C6F4HC2C6H5),.
Determination of the size and charge of dye aggregates in aqueous electrolyte solution
Authors: Craven BR , Griffith JC , Kennedy JG
Published: September 2010

The stability of two dyes
in the presence of electrolyte has been investigated over the period required
for measurement of diffusion coefficients in glass sinter diaphragm cells, and
the results indicate that particle sizes remain constant over such times. The
effect of concentration differences within the cell during a run has been
measured and was found to give rise to considerable error. Corrected diffusion
coefficients have been used together with electrophoretic mobilities to
calculate aggregation numbers and the extent of counter- ion uptake into the
aggregates. The results are shown to be consistent with the ?stack of coins?
model for dye aggregation.
Electron impact studies. XCVII. Acetic anhydride[α,α'-D2]. Synthesis and negative ion molecule reactions. An ion cyclotron resonance study
Authors: Wilson JC , Bowie JH
Published: September 2010

Acetic
anhydride[α,α?-D2] has been synthesized in
near-quantitative yield by the reaction between acetic acid[α-D] and
dicyclohexylcarbodiimide. The gas-phase reaction between the acetate anion and
acetic anhydride[α,α-D2] yields a 1 : 1 adduct which decomposes
by loss of CH2CO and CHDCO so that kH/kD
is 1.2 when the ion- transit time is 10-3-10-4 s, and 2.0
at 10-1-10-2 s.
Some reactions of the trans-Photodimer of 2-methoxynapthalene
Authors: Teitei T , Wells D , Collin PJ , Sugowdz G , Sasse WHF
Published: September 2010

In the absence of base
thermal dissociation of the title compound is accompanied by isomerization to
2?,3-dimethoxy-1,2-dihydro-1,1?- binaphthyl. In the
presence of acid small amounts of 5,6,11,12,-
13,14,15,16-octahydro-5,12:6,11-diethenodibenzo[a,e]cyclooctene-13,16-
dione are also formed. The 14,15-dihydroxy derivative of this ketone is formed
by treatment of the title compound with aqueous potassium permanganate.
Synthesis of β-orcinol meta-depsides
Authors: Elix JA , Norfolk S
Published: September 2010

The total syntheses of the
lichen depsides, decarboxythamnolic, thamnolic, hypothamnolic and haemathamnolic
acid are described.
Sporidesmins. XIV. Modifications to the Opened -S-S- Bridge of Sporidesmin for Coupling to Proteins by Transacylation
Authors: Ronaldson J
Published: September 2010

Alkylation of the opened
-S-S- bridge of sporidesmin formed diethyl secosporidesmin-S,S?-diacetate(3),
dimethyl secosporidesmin-S,S?- diacetate (4), methyl 3-mercaptosecosporidesmin-11a-S-acetate
(5) and methyl 11a-mercaptosecosporidesmin-3-S-acetate (6) which were condensed
with ε-amino groups of poly(L-lysine), bovine plasma albumin and rabbit
serum albumin. The thiol group in compound (6) could not be demonstrated by
conventional tests but its presence was established by its mass spectrum.
The chemistry of 2,1-benzisothiazoles. IX. The reaction of 3-chloro-substituted 2,1-benzisothiazoles with nucleophiles and the preparation of(2,1-Benzisothiazol-3-yl)acetic acid
Authors: Davis M , Homfeld E , McVicars J , Pogany S
Published: September 2010

3-Chloro-2,1-benzisothiazole
(2; R = H, R? = Cl) and 3,5-dichloro-2,1- benzisothiazole (2;R,R? = Cl)
react readily with nucleophiles, and yield 3-substituted products. Acid
hydrolysis of one such product, ethyl (2,1-benzisothiazol-3-yl)cyanoacetate (2;
R = H, R? = CH(CN)CO2Et),affords (2,1-benzisothiazol-3-yl)acetic
acid (2; R = H, R? = CH2CO2H), an auxin
analogue.
Double alkoxides of zirconium with alkaline earth metals
Authors: Govil S , Mehrotra RC
Published: September 2010

Volatile double
isopropoxides M[Zr2(OPri)9]2
and MZr3(OPri)14 of
zirconium with alkaline earth metals (M = Mg, Ca, Sr
or Ba) are described. Their likely structures are
discussed on the basis of alcoholysis studies, molecular weights, i.r. and N.M.R. spectra.
Substituted endo-Tricyclo[3,2,1,02,4]oct-6-enes. III. 1H N.M.R. spectra
Authors: Kagi RI , Johnson BL
Published: September 2010

The 1H n.m.r,
spectra of some endo-tricyclo[3,2,1,02,4]oct-6-enes and
endo-tricyclo[3,2,1,02,4]-octanes have been measured and analysed.
Correlations between structure and chemical shifts as well as structure and
coupling constants have been examined.
Acetyllasiocarpine, an alkaloid from Heliotropium europaeum
Authors: Culvenor CCJ , Johns SR , Smith LW
Published: September 2010

A new minor alkaloid of Heliotropium europaeum has been
identified as an acetyllasiocarpine with the acetyl group on the β-hydroxyl
of the lasiocarpic acid moiety. ��� Proof of structure is provided by 13C
nuclear magnetic resonance data. The alkaloid is formed by mild acetylation of
lasiocarpine.
The reductive halogenation of aromatic azo compounds
Authors: Wilkinson BD , Happer DAR
Published: September 2010

The conversion of compounds
of the type Ar-N=N-Y into p-X-ArNHNHY
by the reaction with hydrogen halides has been re-examined and has been found
to be not as general a reaction as expected. The most likely mechanism is one
involving nucleophilic addition of halide ion to the aromatic nucleus at the
position para to the azo group, this being facilitated by the strong -R
character of the -N=N-YH+ substituent. This addition is made
essentially irreversible by a series of prototropic shifts resulting in the
formation of a stable hydrazo compound.
The crystal structure of Hexakis(2-pyridone)copper(II) perchlorate
Authors: Taylor D
Published: September 2010

Crystals of
hexakis(2-pyridone)copper(II) perchlorate, [Cu(C5H5NO)6]
(ClO4)2, are monoclinic, a 9.453(2), b 10.492(3), c
17.794(4) Ǻ, β 95.57(2)�, space group P21/c with Z = 2.
The structure was solved by Fourier methods using X-ray diffractometer data and
refined by block-diagonal least-squares to convergence at R 0.037, Rw
0.044 for 3054 independent reflections. The octahedral coordination of the
copper atom in the centrosymmetric cation is tetragonally distorted with Cu-O
bond lengths of 1.922(2), 1.952(2) and 2.546(2) Ǻ. The ligands are in the
pyridone tautomeric form and coordinate the copper atom through the exocyclic
oxygen atoms. There are N-H...O bonding interactions between the ligands in the
equatorial plane and the axial ligands (N...O distances of 2.781(3) and
2.894(3) Ǻ). The perchlorate ions (Cl-O,
1.412-1.436 Ǻ) are hydrogen-bonded to the N-H groups of the axial ligands
(N...O 2.958 Ǻ.
Paramagnetic anisotropy and electronic structure of copper(II) tetraphenylporphin
Authors: Murray KS , Sheahan RM
Published: September 2010

Magnetic anisotropy
measurements have been made on copper(II) tetraphenylporphin over the
temperature range 300-100 K. The sign of the anisotropy is consistent with the unpaired
electron being in a dxy orbital (where the x and y directions are
between the adjacent nitrogen donor atoms). The temperature dependence of the
principal molecular susceptibilities can only be explained by assuming a large
second-order Zeeman term. The ligand-field parameters
deduced from the present measurements are different from those obtained by
e.s.r. studies, and reasons for these differences are discussed. The general
application of magnetic anisotropy measurements to planar copper chelates is
critically evaluated.
Synthesis and rearrangements of 1,2,2,4,4,-Pentamethylbicyclo[1,1,0]butane
Authors: Hamon DPG
Published: September 2010

The synthesis of the title
compound (3) by the intramolecular displacement of alkoxide ion is reported.
Acid-catalysed rearrangement of (3) gave 2,3,5-trimethylhexa-l,4-diene (9),
2,3,5-tri- methylhexa-2,4-diene (10) and 2,4,5-trimethylhexa-1,4-diene (11) in
the ratio of c. 3 : 3 : 7 respectively. Pyrolytic rearrangement of (3), in the
vapour phase in the presence of triethylamine, gave the same products but the
ratio of (9) to (11) was 3 : 1. This change in the ratio of (9) : (11) is
consistent with an initial non-concerted cleavage of the bicyclobutane to give
diradical species.
Removal of the C 4 methyl groups from triterpenoids. Conversion of lanosterol into 14α-Methylcholesta-4,8-dien-3-one and the modification of ring A of methyl glycyrrhetinate
Authors: Cohen KF , Pinhey JT
Published: September 2010

14α-Methylcholesta-4,8-dien-3-one
(9a) has been synthesized from lanosterol by a route involving the ?abnormal?
Beckmann rearrangement of the oxime of 5α-lanost-8-en-3-one to the
3,4-seco nitrile (1a), from which the steroidal ring A was formed via the 3,5-dioxo
4,5-seco intermediate (8a). The formation of (8a) from the seco
nitrile (1a) was readily achieved in a high-yielding sequence, which entailed
stepwise degradation of the isopropenyl group, protection of the introduced 5- oxo function, and reaction of the cyano group with a
Grignard reagent.

The application of the above route to the
modification of ring A of methyl glycyrrhetinate has also been investigated.
Although the required triketone (8b) could be obtained, the method was rather
low- yielding due to attack by the Grignard reagent on (11b) occurring at both
C3 and C 11.
The hydrazinolysis of heterocyclic compounds. III. 5-Substituted 6-Amino-4-hydroxy-1-methylpyrimidine-2(1H)-thione
Authors: Dickinson RG , Jacobsen NW
Published: September 2010

6-Amino-4-hydroxy-1-methylpyrimidine-2(1H)-thione,
as well as its 5- nitroso and 5-amino derivatives, reacts with hydrazine to
yield 4- amino-5-hydrazino-1,2,4-triazole-3-thiol and (4-amino-5-mercapto-1,2,4-
triazol-3-yl)acetohydrazide as common products. A preliminary reductive
sequence C5-NO → -NH2 → -H is indicated.
The synthesis of pinpollitol (1,4-Di-O-methyl-D-chiro-inositol)
Authors: Angyal SJ , Gallagher RT , Pojer PM
Published: September 2010

Pinpollitol, a new cyclitol recently
isolated from Pinus radiata, has
been synthesized and its structure proven to be 1,4-di-O-methyl-D-chiro-inositol.
Stobbe-type condensation involving diethyl diglycollate
Authors: El-Newaihy MF , Salem MR , El-Bassiouny FAA
Published: September 2010

Benzaldehyde, p-anisaldehyde,
acetophenone and acetone condense with diethyl diglycollate in the presence of sodium hydride to give
fairly good yields of the corresponding half-esters. With benzaldehydeand p-anisaldehyde the (Z)-half-esters (2a)
and (2b) predominated. Condensation with benzophenone
was only effected with potassium t-butoxide in
boiling t-butyl alcohol. The structure and configuration of the half-esters was
established by chemical and spectroscopic evidence.
The occurrence of senkirkine in Tussilago farfara
Authors: Culvenor CCJ , Edgar JA , Smith LW , Hirono I
Published: September 2010

The medicinal herb, Tussilago farfara L.,
is shown to contain the hepatotoxic pyrrolizidine alkaloid, senkirkine.
A binuclear rhodium(III) dithiocarbamate complex, [Rh2(Me2NCS2)5] BF4
Authors: Hendrickson AR , Martin RL , Taylor D
Published: September 2010

Attempts to prepare the
reported rhodium(1V) dithiocarbamate complex [Rh(Me2NCS2)3]
BF4 have yielded instead a new binuclear rhodium(111) cation, [Rh2(Me2NCS2)5]+,
which has been characterized by chemical, spectroscopic and X-ray structural
techniques. The relationshipbetween the recently
reported structural types for [M2(R2NCS2)5]*
species is discussed.
Studies on unsaturated sugars with particular reference to the synthesis of 6-Deoxy-6-fluoro derivatives
Authors: Blackburne ID , Fredericks PM , Guthrie RD
Published: September 2010

Three fluoro-substituted
unsaturated sugars have been synthesized by transformations within the D-glucal and ethyl 2,3-dideoxy-α-D-erythro-hex-2-enopyranoside
series. A number of the intermediate unsaturated sugars not previously
described have been characterized. The advantages of the t-butyldimethylsilyl
blocking group in such syntheses are described.
Bisnitrosomenthone
Authors: Carman RM , Saraswathi GN , Verghese J
Published: September 2010

Spectral comparisons
between the bisnitroso derivatives of chiral and racemic menthone show that the bisnitroso
derivative of racemic menthone
is meso
rather than racemic.
New Group IB metal chemistry. VII. Reactions between copper arylacetylides and some iridium(I) and rhodium(I) complexes
Authors: Salah OMA , Bruce MI
Published: September 2010

The hexanuclear cluster
complexes Ir2Cu4(C2Ar)8(PPh2R)2
(Ar = Ph, C6H4Me-p, C6H4F-p
or C6F5, R = Ph; Ar = Ph or C6F5,
R = Me) are formed in reactions between IrCl(CO)(PPh2R)2
and CuC2Ar. The rhodium analogues Rh2Cu4(C2Ar)8(PPh2R)2
(Ar = Ph, C6H4Me-p,
C6H4F-p or C6F5; R = Ph or Me) were
obtained with RhC1(CO)(PPh2R)2 or RhC1(PPh3)3
(Ar = C6F5 only).From two of the reactions,
IrCu3(C2Ph3)3 and IrCu(C2C6F5)4/PPh3)3
were also isolated. Further reactions of
the clusters with Fe2(C0)9 have given the octanuclear complexes Ir2Cu4Fe2-(C2Ar)8(C0)8(PPh3)2(Ar=Ph or C6H4Me-p).
Ethylxanthates of phosphorus(III), arsenic(III), antimony(III) and bismuth(III)
Authors: Winter G
Published: September 2010

The infrared and
ultraviolet spectra of phosphorus(111), arsenic(111), antimony(111) and
bismuth(111) ethylxanthates are compared. The C-O
band position (around 1200 cm-l) decreases monotonically (7 cm-1
intervals) from phosphorus to bismuth. The absorptions in the ultraviolet are
assigned to intraligand and charge-transfer bands.
Bismuth ethylxanthate dissociates appreciably in alcoholic solution. The
tetrakis(ethy1xanthate) ions of antimony(111) and bismuth(111) were isolated as
their tetraethylammonium salts.
Annelation of organoboranes derived from geraniol
Authors: Murphy R , Prager RH
Published: September 2010

Alicyclic products have
been obtained from geraniol derivatives in four ways: carbonylation of the
intermediate borane either by treatment with carbon monoxide under pressure or
by rearrangement of the cyanoborate under the influence of an electrophilic reagent;
coupling under the influence of alkaline silver nitrate or by rearrangement of
the bromo derivative obtained by photochemical bromination. The methods are
compared and the nature of the products studied.
P.M.R. spectra of heteroaromatic molecules containing bridgehead nitrogen atoms. I. Tetrazolo[1,5-a]quinoline and 5-Methyltetrazolo[1,5-a]quinoline
Authors: Heffernan ML , Irvine GM
Published: September 2010

This paper is the first of
a series dealing with the analysis of the 100-MHz p.m.r,
spectra of hetero-aromatic molecules containing a bridgehead nitrogen atom as
part of the conjugated system, e.g. pyrrolo[l,2-a]quinoline. The spectra of the aza-substituted
derivatives tetrazolo[l,5-a]quinoline
and 5-methyltetrazolo[l,5-a]quinoline in Me2SO
and CDCl3 solutions are analysed in detail. Special attention was
directed to the determination of the long-range inter-ring coupling constants
and their relative signs by multiple-resonance techniques. The analysis of the
spectrum of the 5-methyl compound was considerably simplified by decoupling of
the methyl protons from the remainder. Evidence was found for a five-bond
long-range coupling constant, J4,6, and a seven-bond coupling
constant, J4,8 both having a magnitude around 0.3 Hz. Selective
double and triple resonance experiments indicated that the relative sign of
both of these long-range coupling constants was positive.
P.M.R. spectra of heteroaromatic molecules containing bridgehead nitrogen atoms. IV. Pyrrolo[1,2-a]quinoxaline
Authors: Heffernan ML , Irvine GM
Published: September 2010

The complex eight-proton p.m.r, spectra of pyrrolo[l,2-a]quinoxaline in (CD3)2SO and CDC13
solutions were fully analysed. Evidence for non-zero inter-ring coupling
constants was obtained by detailed comparison of the experimental and
theoretically simulated spectra. Approximate chemical shifts for pyrrolo[l,2-alquinoxaline in CCl4, (CH3),C0,
CH3COOH, CF3COOH and C6D6 were also
obtained.
P.M.R. spectra of heteroaromatic molecules containing bridgehead nitrogen atoms. V. Pyrrolo[a]quinoline
Authors: Heffernan ML , Irvine GM
Published: September 2010

The p.m.r.
spectra of (CD3)2SO and CDCl3 solutions of pyrrolo[a]quinoline, a nine-spin
system, have been analysed. In the former case, the various multiplets
were sufficiently non-overlapping for detailed double-irradiation experiments
to be performed in order to confirm the proton assignments and to determine the
magnitudes and relative signs of several inter-ring coupling constants. For the
CDCl3 solution, it was found that there was broadening of the
five-membered ring proton resonances at ambient temperature. A
variable-temperature study showed that the broadening was arising from the
exchange of the H1 and H3 protons and that the effects of exchange could be
avoided by running the spectra at or below -20�.
The mechanism of reaction of phosphoramidate monoanions with nucleophiles
Authors: Baker JR , Lawlor JM
Published: September 2010

The kinetics of reaction of
the N-(4-chlorophenyl)phosphoramidate monoanion in hydroxylamine buffer require
an intermediate common to hydrolysis and hydroxylaminolysis. The intermediate is
possibly an induced-dipole pair analogous to the ion pairs suggested for
substitution at saturated carbon. The same type of intermediate may be a
feature of the reactions of all phosphoramidate monoanions and of phosphate
monoester monoanions and dianions.
Behaviour of some sulphur-nitrogen compounds in disulphuric acid
Authors: Bali A , Malhotra KC
Published: September 2010

Thiotrithiazyl chloride and thiodithiazyl chloride form S4N3+ and S3N2+ ions when dissolved in
disulphuric acid. Tetrasulphur tetranitride forms S82+, S2N2+, NH4+, SO2 and NH2SO2OH when
dissolved in disulphuric acid. From conductance and cryoscopic studies, it is not possible to write
an overall stoichiometric reaction for its dissolution.
β-Methylation shifts from the 13C N.M.R. spectrum of 1,4-O,O-Dimethyl-chiro-inositol
Authors: Blunt JW , Munro MHG , Paterson AJ
Published: September 2010

The carbon resonances of
1,4-0,O-dimethyl-chiro-inositol are assigned and the β-methylation shifts
ascertained. The relationship between chemical shift and the stereochemistry of
the methoxyl carbons is also examined.
Trimeric products from the free radical oxidation of (Z)-isoeugenol
Authors: Miller IJ
Published: September 2010

Four trimeric
oxidation products have been isolated from the reaction between isoeugenol and tri-t-butylphenoxyl
radical in methanol, and structures for these have been proposed on the basis
of their proton magnetic resonance and mass spectral properties. All linkages
were those expected from radical coupling, and one of the products was an
acetal. Thus a route to the formation of ketones in lignin is demonstrated.
Photo- and electro-chemical processes at organic crystal electrodes. III. Hole photo-injection into anthracene single crystals
Authors: Lyons LE , McGregor KG
Published: September 2010

Adsorption to an organic
substrate by a suitable reducible solute influences the magnitude of the hole
saturation photo-current and hence the charge-carrier injection efficiency.
Efficiencies up to 0.65 have been observed with organic photo-injectors, and 0.31
for a hexacyanoferrate(111) hole photo-injector in
the singlet region of anthracene (λ 395 nm).
About 5 � 4% of the holes formed in the initial photo-injection do not reach
the external circuit, presumably because they react at the injecting surface.
Effect of dose rate on the radiation graft copolymerization of styrene to cellulose in the presence of acid
Authors: Garnett JL , Phuoc DH , Airey PL , Sangster DF
Published: September 2010

At both low and high dose
rates (19.5-501 krad/h), in the absence of air, the
presence of certain mineral acids enhances the grafting of styrene in methanol
to cellulose by the mutual irradiation technique. Sulphuric
acid is the most effective of the mineral acids in enhancement. In the presence
of air, acid enhances grafting at high dose rates (c. 400 krad/h).
Acid can also induce a Trornmsdorff peak in the
grafting system or, alternatively, enhance the magnitude of the effect if it is
already present. These enhanced acid
effects in radiation grafting to cellulose are attributed to an increase in
hydrogen atom yields.
The reactions of acetylenic esters with N-substituted indoles
Authors: Shandala MY , Al-Jobour NH
Published: September 2010

Reaction of an arylpropiolic ester with indol-1-ylacetamide and ethyl
indol-1-ylacetate in the presence of sodium ethoxide
yielded 4-aryl-3-(indol-1-yl)pyridine-2,6(1H,3H)-diones and
ethyl arylpropioloyl- (indol-1-yl)acetates
respectively. Reaction of arylpropiolic esters with
1-acetylindole in the presence of sodium ethoxide at 0�
yielded two products, 5-aryl-1-(indol-1-yl)pent-4-yne-1,3-dione and ethyl
8-(indol-1-yl)cinnamates, as a result of Claisen and
Michael reactions respectively. These products were identified on the basis of
spectral and analytical data.
Carbonyl halides of the Group VII transition metals. V. Derivatives of manganese halocarbonyls with Bis(diphenylarsino)methane
Authors: Colton R , McCormick MJ
Published: September 2010

The reactions between
Mn(CO)5X(X = Cl, Br) and bis(diphenylarsino) methane, dam, have been studied. The most
surprising feature of the system is the lack of complexes of the type [Mn(CO)3(dam)X].
Binuclear complexes [Mn2(CO)6(dam)X2] dominate
the system and these show unusual disproportionation
to Mn0 and Mn11. The reactions with the corresponding ditertiary phosphine, dpm, are
much simpler and no binuclear complexes were observed. Infrared and N.M.R.
studies have helped to elucidate the structures of the compounds prepared.
Photochemical reactions of azo compounds. XVII Photoinduced reaction of 2,2,4,4,-tetrachloroazobenzene with acetyl chloride
Authors: Lewis GE , Mayfield RJ
Published: September 2010

The photoinduced
reaction of 2,2',4,4'-tetrachloroazobenzene with acetyl chloride has been found
to give an unexpected mixture of products, incorporating only a relatively poor
yield of the predicted main product, N,N
'-diacetyl-2,2',4,4',6-pentachlorohydrazobenzene. It has been found, moreover,
that the latter compound in aqueous methanolic potassium hydroxide, in addition
to yielding the expected hydrolysis/oxidation product,
2,2',4,4',6-pentachloroazobenzene, undergoes an interesting side reaction which
regenerates 2,2',4,4'-tetrachloroazobenzene.
Mass spectral studies of lanthanide chelates. II. Lanthanide chelates of three fluorinated β-diketones
Authors: Livingstone SE , Zimmermann WA
Published: September 2010

The lanthanide chelates
MetL3,nH2O (Met = Pr, Nd, Sm, Eu, Gd,
Dy, Ho, Er, or Yb; L = PhCO= CHCOCF3,
p-MeC6H4CO=CHCOCF3,
p-MeOC6H4CO=CHCOCF3;
n = 2, 3 or 1) have been isolated. The conditions were found to be critical,
involving the slow addition of an ammoniacal aqueous
alcoholic solution of the β-diketone to an excess of the lanthanide
nitrate solution while the pH was maintained within the range 6.0-6.5. The mass
spectra of most of the chelates were obtained and were essentially similar and
fluorine migration to the metal was found to occur. Although a peak for the ion
M-L (M = MetL3+) is present in the spectra, peaks for M-2L and M-3L
are absent; however, peaks were obtained for the ions M-2L+ F and M-3L+2F (Met111F2).
A peak for the ion M- L+ F (Met11F) was obtained when Met = Sm, Eu and Yb.
The valency change from 3 to 2 occurring in the mass
spectrometer in the case of samarium, europium and ytterbium is in accordance
with their chemical behaviour in solution.
Photochemical syntheses. XI. X-Ray analysis and molecular structure of 1,8-Diphenyl-1a,2,7,7a-tetrahydro-1,2,7-metheno-1H cyclopropa[b]naphthalene, a naphthalene-diphenylacetylene photoadduct
Authors: Kowala C , Poppleton BJ , Sasse WHF
Published: September 2010

The structure of the title
compound(1) has been confirmed by X-ray crystal structure analysis.
Naphthalene-1,3,8-triol
Authors: Cameron DW , Sidell MD
Published: September 2010

One of the two compounds
described in the literature as naphthalene-1,3,8-triol is
6,8-dihydroxy-3,4-dihydronaphthalen-l(2H)-one. It may be converted into
naphthalene-1,3,8-trio1 by a brominationdehydrobromination procedure.
Crystal structure of cis-Tetracarbonylbis(chloromercury)iron
Authors: Raston CL , White AH , Wild SB
Published: September 2010

The crystal structure of
the title compound has been determined by direct methods from X-ray diffraction
data and refined by least squares to a residual of 0.071 for 2647 'observed'
reflections. Crystals are monoclinic, C2/c, a
= 36.81(1), b = 11.181(2), c = 20.369(5) �, β = 95.28(3)�, Z =
32. There are four independent molecules in the asymmetric unit, all with the cis disposition of ligands (<Fe-Hg),
2.498 �; <Hg-Fe-Hg), 80.9�); in one of the molecules one of the
carbonyl sites is occupied by a more substantial moiety, possibly a result of
partial occupancy of HgCl as a result of disorder or
decomposition.
The total synthesis of (±)-α-Amorphene
Authors: Gregson RP , Mirrington RN
Published: September 2010

The first total synthesis
of the sesquiterpene hydrocarbon (+)-α-amorphene
(zizanene) (1) has been achieved. A unique feature of
the synthetic scheme is the introduction of all three chiral
centres in

one step by an oxy-Cope rearrangement.
Kinetics of aquation and base hydrolysis of the macrocyclic complex trans-Bromo(N-meso-5,12-dimethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)nitro-cobalt(III) perchlorate
Authors: Lawrance GA , Hay RW
Published: September 2010

The macrocyclic complex trans-[Co(dtcd)(NO2)Br]
[ClO4] (dtcd =
5,12-dimethyl-l,4,8,1l-tetraaza-cyclotetradeca-4,ll-diene) has been prepared
and its hydrolysis kinetics investigated. At 25�C and 0.1 M HN03 the
aquation occurs with kaq
= 6.2 x 10-3 s-1 to give the trans-Co(dtcd)(NO2)- (OH2)]2+
cation. The activation parameters at 298 K are ΔH? = 75.0 kJ mol-1
and ΔS? = -35.6 J K-1 mol-1. Hydrolysis of the
bromide in the pH range 7.5-8.8 follows the rate expression kobs = kaq + kOH[OH-].
At 25�C (I = 0.1 M, NaClO4) kOH
= 1.21 x 103 1. mol-1 s-1 with the activation
parameters for base hydrolysis being ΔH? = 74.2 kJ mol-1 and ΔS?
= +63.2 J K-1 mol-1 at 298 K. Aquation
and base hydrolysis of the bromo complex at 25�C occur at rates 14 and 5 times
faster respectively than those previously reported for the analogous trans-[Co(dtcd)(NO2)Cl]+ complex, the acceleration being due to a
more favourable entropy of activation in each case.
Conformations of some highly substituted ethanes in solution
Authors: Huang HH
Published: September 2010

The dehydrogeno-dimers
of 2,6-dichlorotoluene, benzyltrimethylsilane, p-chlorobenzyltrimethylsilane, anthrone,
xanthen, phthalide and α-tetralone have been
prepared by free-radical dimerization, and their conformations examined with
the aid of electric dipole moment and infrared measurements.
Substituent effects by 19F nuclear magnetic resonance: Polar and π-electron effects
Authors: Adcock W , Gupta BD , Khor T
Published: September 2010

A number of model
substituted bicyclic aryl fluorides, including three new
fluorobenzocycloalkenes, have been synthesized and their fluorine- 19 spectra
measured. An analysis of the data leads to the important conclusion that
electrostatic-field effects play an important role in determining aryl 19F
chemical shifts. Further the relative π-electron distributions of several
benzocycloalkenes are indicated.
The effect of steric hindrance on the SRN1 reaction of some α-Alkyl-p-nitrobenzyl chlorides
Authors: Norris RK , Randles D
Published: September 2010

The reactions of a series
of α-substituted p-nitrobenzyl chlorides, p- NO2C6H4CH(Cl)R (R = Me, Et, Prt,
But), with the lithium salt of 2- nitropropane
in dimethyl sulphoxide and dimethylformamide have been studied. When R = Me or
Et, competing SRN1 and SN2 processes take place, giving
C- and O-alkylated products respectively. In the more sterically hindered cases
where R = Pri or But, the only
reaction taking place has been shown to be an SRN1 reaction with
exclusive O-alkylation. These observations indicate that the SRN1
reaction is prone to steric hindrance, and that radical alkylation of the
ambident nitronate ion occurs on the more accessible oxygen atom in sterically
hindered situations.
Diazepines. XXI. The mass spectra of 2,3-Dihydro-1,4-diazepinium salts
Authors: Lloyd D , McNab H , Marshall DR
Published: September 2010

The mass spectra of a
series of 2,3-dihydro-1,4-diazepinium salts have been recorded. The commonest
breakdown pattern involves initial loss of an N1-C2 fragment.
The chemical constituents of Australian Flindersia species. XXII. Some extractives of F. brassii
Authors: Nimgirawath S , Ritchie E , Taylor WC
Published: September 2010

From the bark of Flindersia
brassii Hartley & Hyland, a new substance, flinderbrassin, C31H40O12,
m.p. 215°, [α]18D -8.2°,
was isolated; it was reserved for further study. The leaves gave a very small yield
of brassilignan, shown to be the known (-)-trans-3,4-bis(3,4- dimethoxybenzyl)tetrahydrofuran.
Bond-stretch isomerism in [2,2,2]propellanes
Authors: Gregory AR , Paddon-Row MN , Radom L , Stohrer W
Published: September 2010

The possible existence of
bond-stretch isomers for the system 1-aza-4- boratricyclo[2,2,2,01,4]octane
(abto) ↔ 1-aza-4-borabicyclo[2,2,2]octane (abbo) has been investigated by using molecular orbital
theory at the PMO, EHT, CNDO, INDO and ab initio
levels. As a consequence of the interplay between through-space and
through-bond interactions, the stretching of the central bond is accompanied by
an intended but avoided crossing between an occupied and a virtual molecular
orbital. The closed (abto) and open (abbo) forms are therefore expected on the basis of
conventional orbital symmetry arguments, to be separated by a potential energy
barrier. Our ab initio calculations suggest that the
barrier separating abto and abbo
is small, with the latter being the more stable isomer. These results may be
rationalized in terms of the disparity in the energies of the 2p atomic
orbitals of boron and nitrogen which weakens their direct stabilizing
interaction in abto. Calculation shows abto to be more polar than abbo
and the dipole moment reverses direction during the bond-stretching process.
The effect of solvent and substituents on the bond-stretch equilibrium is
discussed.
High acidity disulphonyl carbon acids
Authors: Ang KP , Lee TWS
Published: September 2010

Four disulphonyl carbon
acids, (PhCH2SO2)2CHY (Y = H, Ph,p-CNC6H4,p-
NO2C6H4), have been synthesized and their
ionization constants determined by spectrophotometric measurements in 80% (w/w)
dimethyl sulphoxide- water at 25�C. The pKa values, ranging from 11.65�0.02
to 7.75�0.02, present strong evidence for the conjugative effect of the two
sulphonyl groups attached to the carbon acids.
Organophosphorus compounds. P-Arylated perhydro-1,2-azaphosphorines
Authors: Hewitt DG , Newland GL
Published: September 2010

Treatment of ethyl
4-bromobutylphosphonochloridate with phenylmagnesium bromide, followed by
acid-catalysed hydrolysis of the product, gave 4- bromobutyl(phenyl)phosphinic
acid. This was converted into the corresponding phosphinamide by treatment with
thionyl chloride and then with aqueous ammonia. Cyclodehydrobromination with
sodium hydride in warm xylene then gave a good yield of 2-phenylperhydro-1,2- azaphosphorine
2-oxide. Some other routes to this compound were investigated.
The preparation of α-hydroxymethylserine
Authors: O'Conner MJ , Brush JR , Teo S
Published: September 2010

Convenient methods for the
preparation of α-hydroxymethylserine in high yield by the treatment of the
copper(II) complex of dihydro-1H,3H,5H- oxazolo[3,4-c]oxazole-7a-carboxylic
acid with hydrogen sulphide or by catalytic hydrogenation of the complex are described.
Thermodynamics and mechanism of hydrophobic interaction
Authors: Oakenfull DG , Fenwick DE
Published: September 2010

.In the mixed solvent, 0.1 mole fraction ethanol-water, long-chain decyltrimethylammonium carboxylates
form ion pairs. Ion-pair association constants (and hence the free energy of ion-pair formation)
can be measured conductometrically. It is possible to separate the hydrophobic from the electrostatic
contribution to the free energy of ion-pair formation by systematically varying the hydrocarbon chain
length.
We report measurements of the free energy of hydrophobic interaction (ΔG°HI) over the temperature
range 278-328 K. The value of ΔG°HI becomes more negative (stronger hydrophobic interaction)
with increasing temperature. The temperature coefficient of ΔG°HI was used to calculate the enthalpy
(ΔH°HI) and entropy (ΔS°HI) of hydrophobic interaction. At low temperature the entropic contribution
to the free energy is the larger but ΔH°HI, dominates at temperatures above c. 324 K.
The volume change of hydrophobic interaction was similarly estimated from the volume change of
ion-pair formation. We obtained values of apparent molar volume of the decyltrimethylammonium
carboxylates (over a range of concentrations) from very precise density measurements. These could
then be combined with the appropriate ion-pair association constant (from the conductance measurements)
to give the partial molar volumes of the free ions and the ion pair. Hydrophobic interaction
was found to be accompanied by a substantial increase in volume amounting to 10.2 ± 0.3 ml mol-1
for each pair of interacting methylene groups.
Our results support the view that hydrophobic interaction occurs with a further ordering of water
molecules over and above that which exists in the hydrophobic hydration layer surrounding an isolated
hydrophobic molecule.
The infrared, Raman and ultraviolet spectra of phthalonitrile, terephthalonitrile and 2,6-dichlorobenzonitrile
Authors: Barraclough CG , Bissett H , Pitman P , Thistlethwaite PJ
Published: September 2010

The solid-phase infrared
(0-4000 cm-1) and Raman spectra, and the gas- phase ultraviolet
spectra, of phthalonitrile, terephthalonitrile and 2,6-dichlorocenzonitrile have
been measured and an assignment made. The ultraviolet spectra of all three
compounds, particularly terephthalonitrile, are rather diffuse. For
phthalonitrile, the ultraviolet spectrum has a large forbidden character with
most of the intensity associated with vibronically induced transitions.
The crystal and molecular structure of a platinum-silatrane complex
Authors: Scollary GR
Published: September 2010

A structural analysis of
the platinum-silatrane complex, PtCl [Si(OCH2CH2)3N] [PMe2Ph]2,
has been carried out by X-ray diffraction. Crystals are monoclinic, space group
P21/c, a 6.630(4), b 17.465(6), c 22.297(6) Ǻ, β 97.4(2)�,
Z 4. The structure has been refined by a full- matrix least-squares procedure
to R 0.048 for 2165 reflections. Basic geometries are square (platinum),
tetrahedral (silicon) and trigonal (nitrogen). Within the silatrane ligand, the
Si-N non-bonding distance is 2.89(1) Ǻ.
Rearrangements of ethylene oxide derivatives. Stereoselectivity of the prochiral C1 hydrogens in the boron trifluoride catalysed rearrangement of 1,2-epoxyoctane
Authors: Coxon JM , Lim C
Published: September 2010

The boron trifluoride
catalysed rearrangement of 1,2-epoxyoctane to give octanal proceeds by selective
(c. 1.4 : 1) migration of the prochiral hydrogen trans to the alkyl group.
Synthesis of emodin methyl ethers
Authors: Cameron DW , Crossley MJ
Published: September 2010

Procedures are summarized
for the conversion of emodin (1) into all possible mono- and di-methyl ethers.
The 1-methyl ether (2) is characterized for the first time. The 1- and 8-methyl
ethers are differentiated by small differences in the chemical shifts of
appropriate aromatic protons of their respective 6-benzoates.
The infrared spectrum of isotopically diluted potassium hydrogen bifluoride. Doubling of the HF stretching and of the v3 + v1 band
Authors: Spinner E
Published: September 2010

Infrared spectra (of mulls
in Nujol and Fluorolube and discs in potasium iodide)
have been obtained for crystalline KDF2 of higher deuterium content
(c. 97.5%) than used by previous workers. This made possible an unambiguous
identification of the bands of KHF2 as a solid solute in KDF2.
HF stretching (v3) is split into a doublet with separation c. 52 cm-1,
and the combination band v3 + v1 has a doublet separation
of c. 64 cm-1. For 1.5% KDF2 in KHF2 the
splitting of v3 of DF2- is too small to
produce two separate bands. The splitting is attributed to the interconversion
doubling which Ketelaar erroneously believed to have detected in 1941.
Arguments previously put forward against the F-...HF structure are
shown not to take into account the increasing tendency of the anionic dipoles
to adopt an ordered arrangement as the temperature is lowered. ��� KHF2 and KDF2 have
also been examined in solid solution in potassium halides and in water. Narrow
v3 bands are obtained in KCl and KBr, but broad ones, as in crystalline KHF2, in
KI and in water.
Crystal structure of a natural potassium-barium hexatitanate isostructural with K2Ti6O13
Authors: Bagshaw AN , Doran BH , White AH , Willis AC
Published: September 2010

The crystal structure of a
mineral with the stoichiometry (K0.58Ba0.36)2(Ti0.93FeIII0.06)6O13
has been determined by X-ray diffraction and refined by full-matrix least
squares to a residual of 0.076 for 1688 ?observed? reflections. Crystals are
monoclinic, C2/m, a = 15.453(2), b = 3.8368(7), c = 9.123(2) Ǻ,β = 99.25(1)�, Z = 2, and are isostructural
with the (Na,K,Rb)2Ti6O13
family. High-resolution electron microscopy has confirmed that the Ba and FeIII species
(the latter in a high-spin state) are randomly substituted for K and Ti
respectively.
New chemical constituents of Planchonia careya
Authors: Khong PW , Lewis KG
Published: September 2010

From the ether extract of
the bark of Planchonia careya
there have been isolated 16-deoxybarring-togenol C, barringtogenol C and the
previously unreported 16α,21β,22α,28-tetrahydroxyolean-12-en-3-one.
The methanol extract, after mild acid hydrolysis, gave the same three compounds
together with three new esterified triterpene glycosides, the structures of
which have been elucidated.
The chemistry of pyrrolic compounds. XXXVII. Monobenzoporphyrins: The rhodoporphyrin of petroleum deposits
Authors: Clezy PS , Fookes CJR , Mirza AH
Published: September 2010

A monobenzoporphyrin has
been prepared from porphyrin derivatives containing a fused cyclo-hexanone
ring. The cyclohexanone system can be constructed either before or after the
porphyrin macrocycle has been synthesized. The spectroscopic properties of the monobenzoporphyrin
are described and these support the proposal that such a species constitutes
the rhodo-type series of porphyrins which have been isolated from some
petroleum deposits.
The temperature dependence of the mobility of aqueous fluoride ion, and the apparent molar volume of sodium fluoride
Authors: Mallanoo T , Stokes RH
Published: September 2010

Conductances of aqueous
sodium fluoride solutions have been measured at 15�, 25� and 45�C to give the
limiting mobility of fluoride ion. Apparent molar volumes have been obtained by
means of a continuous dilution dilatometer.
Chemical constituents of Harpullia pendula. II. Further constituents of the bark and leaves
Authors: Cherry RF , Khong PW , Lewis KG
Published: September 2010

Further examination of the
bark of Harpullia pendula
has led to the isolation, from the light petroleum extract, of stigmasterol;
from the ether extract, of a new compound,
15α,16α,22α,28-tetrahydroxy-olean-12- en-3-one, together with
the known triterpenes A1-barrigenol, camelliagenin A and 22α-hydroxyerythrodiol.
From the acetone extract of the bark and the leaves quebrachitol has been
obtained.
Magnetic studies of Hexakis(antipyrene)manganese(II) perchlorate
Authors: Mackey DJ
Published: September 2010

The magnetic anisotropy of Mn(antipyrene)6(ClO4)2
below 20 K indicates that the zero-field splitting parameter (D) is about three
times greater than obtained from e.p.r. measurements
of manganese doped into a series of isomorphous host lattices. Shape anisotropy
effects are significant unless spherical crystals are used. The interpretation
of the magnetic anisotropy above 20 K is complicated by the large diamagnetic
contribution from the ligands and it is suggested that there are significant differences
in the orientation of the ligand molecules in the isomorphous manganese and
magnesium complexes.
Vinylindenes and some heteroanalogues in the Diels-Alder reaction. IV. Reactions of ethenetetracarbonitrile with some 3-vinylindoles
Authors: Bergamasco R , Porter QN , Yap C
Published: September 2010

3-Vinylindoles are
conveniently prepared from methylenetriphenylphosphorane and
indole-3-carbaldehydes. Those studied give normal Diels-Alder adducts with
ethenetetracarbonitrile, except in the case of the 2-methyl derivative, where
steric hindrance results in formation of a cyclobuty-indole. The adducts are
relatively unstable, and decompose rapidly to indolylbutadienetricarbonitriles.
Vapour pressures of some liquids of quasi-spherical molecules near their critical points and the applicability of the principle of corresponding states
Authors: Toczylkin LS , Young CL
Published: September 2010

Vapour pressures of some
liquids of quasi-spherical molecules (CCl4, SiCl4 and GeCl4)
near their critical points are reported. The deviations from the principle of
corresponding states obeyed by the inert gases are calculated by using
Rowlinson's analysis. The magnitudes of the deviations for the tetrachlorides
studied are similar.
Crystal structures of N,N,N',N'-Tetramethylthiuram monosulphide and Diiodo(N,N,N',N'-tetramethylthiuram monosulphide)mercury(II)
Authors: Skelton BW , White AH
Published: September 2010

The crystal structures of
the title compounds, Me2NC(S)SC(S)NMe2 (tmtm) and I2Hg(tmtm),
have been determined by single-crystal X-ray diffraction at 295 K and refined
by full-matrix least squares to residuals of 0.038 and 0.050 respectively for
1080 and 1532 ?observed? reflections. ��� The ligand tmtm is monoclinic, P21/a,
a 14.096(4), b 7.457(3), c 10.178(3)Ǻ, β 110.55(3)�, Z4. The complex
I2Hg(tmtm) is orthorhombic, P212121,
a 12.910(3), b 12.441(3), c 9.863(2) Ǻ, Z4. ��� The structure of the ligand comprises a
pair of planar Me2NCS2 fragments linked at the common
central sulphur atom with a dihedral of 78.4�. As in the related tetraethylthiuram
disulphide, the ?CS2- geometry is very asymmetric:  1.657;
 1.793 Ǻ;  119.3;  115.2;
 125.4�; with C-S-C, 103.2(2)�. The metal-atom geometry in I2Hg(tmtm)
is pseudo-trigonal prismatic, as in I2Hg(Me2NCS2-
S2CNMe2), the prism apex being occupied by a ligand
sulphur atom, but considerable changes are observed in the geometry about the
metal as a consequence of the change in the ligand ?bite?.
Studies in the Cyclopropa-arene series: Approaches to Cyclopropa[a]naphthalene and Cyclopropa[l]phenanthrene
Authors: Chauh TS , Craig JT , Halton B , Harrison SAR , Officer DL
Published: September 2010

Attempted generation of
cyclopropa[a]naphthalene (3b) and cyclopropa[l]phenanthrene (3c) by intramolecular
1,3-elimination from the aryllithium derivatives (2b) and (2c), respectively,
fails. Instead products from organolithium disproportionation reactions are
observed.
Acetolysis and thermolysis of 2-nitrosoiminothiazolidines
Authors: Brown RFC , Colman LJ , Jemison RW
Published: September 2010

2-Nitrosoiminothiazolidine
(1) with acetic anhydride and pyridine gives thiazolidin-2-one,
3-acetylthiazolidin-2-one and 2-thiocyanatoethyl acetate. Thermal decomposition
of (1) and of its 3-methylderivative (2) forms thiazolidin-2-ones.
Crystal structure of o-Phenanthrolinebis(thiourea)copper(I) iodide o-phenanthroline: Stereochemistry of [M(bidentate)(unidentate)2] coordination
Authors: Hall SR , Kepert DL , Raston CL , White AH
Published: September 2010

The crystal structure of
the title compound, [Cu{CS(NH2)2}2(phen)] I,phen, has been
determined by X-ray diffraction with direct methods, and refined by least
squares to a residual of 0.043 for 5383 ?observed? reflections. Crystals are
triclinic, Pī, a 13.263(8), b 12.449(2), c
10.214(2) Ǻ, α 113.20(2), β 90.16(2), γ 112.72(2)�, Z 2.
The coordination about the copper is pseudo-tetrahedral, distorted by the bite
of the phenanthroline ligand [Cu-S, 2.295(2), 2.280(1) Ǻ; Cu-N, 2.072(4),
2.089(5) Ǻ, N-Cu-N, 81.0(2)�; S-Cu-S, 117.31(6)�; N-Cu-S,
107.7(11)-117.23(9)�]. In addition the structure provides the first example of
the determination of the geometry of the uncoordinated o- phenanthro-line molecule.
The stereochemistry of the [M(bidentate)(unidentate)2] coordination
type is considered in terms of a repulsion model.