bluuebunny/crossref_metadata_2025 huggingface dataset:
Dipole moments and conformations of some substituted benzaldehydes
Authors: Bruce EAW , Ritchie GLD , Williams AJ
Published: September 2010

Experimental electric
dipole moments are reported for a number of substituted benzaldehydes (o-, m-,
and p-XC6H4CHO;
X = NO2, CN, F, Br) as solutes in carbon tetrachloride or benzene at
25�C. Analysis of results yields information concerning the preferred conformations
of thesemolecules.
2-Mercaptopyrimidin-4-ol (2-thiouracil) complexes of copper(II), nickel(II), cobalt(II) and iron(III)
Authors: Khullar P , Agarwala U
Published: September 2010

The complexes of
2-mercaptopyrimidin-4-ol with Cu11, Ni11, Co11
and Fe111 have been synthesized.
Their structures have been assigned on the analytical, spectral (i.r, and visible), magnetic and d.t.a.
data. It has been shown that there is a possibility of the Fe-O-Fe bond in the
iron complex.
Structures and thermal decomposition of some diphenyllead bispolyfluorobenzoates
Authors: Cookson PG , Deacon GB , Felder PW , Farquharson GJ
Published: September 2010

The diphenyllead
bispolyfluorobenzoates, Ph2Pb(O2CR)2
(R = C6F5, p-MeOC6F4 or p-EtOC6F4),
obtained from diphenyllead diacetate and the
appropriate polyfluorobenzoic acids, are considered
to have associated structures with bridging bidentate carboxylate groups in the
solid state and to be predominantly monomeric with chelating carboxylate groups
at low concentrations in chloroform. Thermal decomposition of Ph2Pb(O2CC6F5)2
in boiling pyridine gave Ph2Pb(C6F5)2
and a low yield of Ph3PbC6F5, whereas Ph2Pb(O2C-p-MeOC6F4)2
and Ph2Pb(O2C-p-EtOC6F4)2
gave low yields of Ph3Pb-p-MeOC6F4
and Ph2Pb(p-EtOC6F4)2 respectively.
From decomposition of Ph2Pb(O2CC6F5)2
under vacuum, Ph2Pb(C6F5)2, Ph3PbC6F5,
Ph4Pb, PhC6F5, (C6F5)2CO
and CO2 were obtained, whilst Ph4Pb, Ph2, PhR, RCO2Ph, R2CO and CO2
were detected from pyrolysis of Ph2Pb(O2CR)2
(R= p-MeOC6F4
or p-EtOC6F4).
These compounds are formed by competing decarboxylation, rearrangement, and
(under vacuum) homolysis reactions of the diorganolead dicarboxylates, and
by further reactions of the rearrangement products.
An N2O4 isomer as a model for the examination of the origin of the antiferro magnestism of the copper acetate monohydrate dimer
Authors: Harcourt RD
Published: September 2010

Some results of VESCF
molecular orbital calculations, with configuration interaction, are reported
for an N204 isomer having the geometry of

(see diagram in article)

This isomer can mimic the
two copper ions and the oxygen atoms of two acetate ligands of Cu2(O2CCH3)4,2H2O.
The calculations suggest that the primary factor responsible for the singlet-triplet
separation (J ≈ 286 cm-1) for the copper acetate is the
simultaneous overlap which occurs between two lone-pair oxygen atomic orbitals of each acetate ligand with each other and with
the singly occupied orbitals of the copper(11) ions.
The relevance of five-electron three-centre bonding for the interpretation of
the magnetic properties of two classes of binuclear transition metal complexes
is indicated.
Aromatic fluorocarbon mixtures. VI. Vapour pressures of carbon tetrachloride + hexafluorobenzene
Authors: Pasco NF , Fenby DV
Published: September 2010

Measurements are reported
of the vapour pressures of the system carbon tetrachloride + hexafluorobenzene at 278.68 K. The molar excess Gibbs
functions GE/M, obtained from these measurements have been combined with
previously reported molar excess enthalpies to give GE/M at 298 K.
Thermodynamic properties of CCl4+C6F6 at 298 K
are compared with the predictions of liquid mixture theories based on analytic
equations of state.
The AA′BB′ system of conformational populations for derivatives of choline, tryptamine and tyramine
Authors: Culvenor CCJ , Ham NS
Published: September 2010

Equations relating the
magnetic resonance spectral parameters N and L of the AA'BB' system to the
conformational populations of 1,2-disubstituted ethanes
of the type XCH2CH2Y are derived for a variety of
substituents. These equations are used to obtain conformational information for
choline, tryptamine and tyrarnine derivatives in solution.
The reactions of malononitrile with α-diketones and related studies
Authors: Ducker JW , Gunter MJ
Published: September 2010

The reaction of α-diketones
with malononitrile has been shown to give either
simple Knoevenagel adducts or substituted γ-lactams,
depending on the proportions of the reactants used. The behaviour of the adduct
(la) towards nucleophilic attack has been investigated and the resulting
reactions rationalized. The published structures of the products from the
reactions of malononitrile dimer with benzil and from
malononitrile with benzoin have been reassigned.
The absolute configuration of 2- and 3-Isopropyl-γ-butyrolactone
Authors: Kendell M , Wells RJ
Published: September 2010

The absolute configuration
of 2- and 3-isopropyl-γ-butyrolactone has been determined to be (S)-(-).
Mossbauer studies in transition metal chemistry. III. Compounds of iron with some sulphur-containing Schiff base ligands
Authors: Bond M , Martin RL , Roos IAG
Published: September 2010

M�ssbauer spectra are reported for a series of iron complexes
with sulphur-containing Schiff base ligands. These
tridentate ligands are based on the Schiff base formed by the condensation of dithiocarbazic acid and pyridine-2-carbaldehyde and form
complexes with a metal-to-ligand ratio of 1 : 1 and 1 : 2. The M�ssbauer study confirms that most of these complexes
contain iron(11) with examples of both high-and low-spin and one example of a
spin crossover. Several iron(111) complexes were also studied. The quadrupole splittings show the anisotropy in bonding expected for
metal atoms coordinated to different types of atoms within the same chelate
ring. However, for some complexes the splittings are
small, showing that low local symmetries need not produce large electric field
gradients. In cases where it is applicable, the temperature dependence of the
quadrupole splitting has been used to derive a splitting of the t2
and e orbitals produced by the non-cubic symmetry.
For compounds of the form Fe(L)X2, where X is a halide and L the
tridentate ligand, the Mossbauer results are best
interpreted in terms of a five-coordinate structure rather than a
six-coordinate bridged dimer.
Metal derivatives of amide oximes. III. Products of the reaction between dialkyldichlorosilanes and amide oximes
Authors: Goel AB , Gupta VD
Published: September 2010

The reaction of dialkyldichlorosilanes with amide oximes leads to cyclic
products whose monomeric form has an l-oxa-3,5-diaza-2-silacyclopent-4-ene
structure. These compounds exist mostly in adimeric form, occasionally
monomeric or trimeric. Their infrared spectra have
been interpreted. The secondary amino group of the compounds has been
trisilylated.
Organophosphorus compounds. XVI. 2-(N-Dialkylamino)alkyldiphenylphosphines, phosphine oxides and sulphides as analogues of methadone
Authors: Collins DJ , Mollard S , Rose N , Swan JM
Published: September 2010

A series of 2-(N-dialkylamino)ethyldiphenylphosphine
oxides and sulphides was prepared by the addition of a secondary amine to
diphenylvinylphosphine oxide, or the phosphine sulphide, respectively. Similarly,
a series of 2-(N-dialkylamino)propyldiphenylphosphine oxides was prepared from
diphenylprop-1-enylphosphine oxide, or from diphenylprop-2-enylphosphine oxide
which isomerized under the reaction conditions. Reduction of the 2-(N-dialkylamino)propyldiphenylphosphine
oxides with trichlorosilane, and oxidation of the phosphines with sulphur,
afforded the corresponding phosphine sulphides. ��� None of the compounds showed significant
analgesic activity.
Methyleneketenes and methylenecarbenes. II. A new phenolic ring synthesis: 2-Naphthol from o-tolualdehyde
Authors: Brown RFC , McMullen GL
Published: September 2010

Flash vacuum pyrolysis of
2,2-dimethyl-5-(2?-methylbenzylidene)-1,3- dioxan-4,6-dione (1) at 420-620? gives
2-naphthol in 95-100% yield. The reaction probably involves an intermediate 2- methylbenzylideneketene,
which undergoes consecutive [1,5] hydrogen migration and cyclization reactions.
Substituted 2-naphthols and a phenol (biphenyl-3-ol) have been synthesized in a
similar way.
Nickel(II) and copper(II) complexes of the macrocyclic ligand 5,7,7-Trimethyl-1,4,8,11-tetraazacyclotetradec-4-ene
Authors: Curtis NF , Milestone TN
Published: September 2010

Nickel(II) and copper(II)
complexes of 1,4,8,11-tetraazaundecane, (L), react with acetone, diacetone
alcohol or mesityl oxide to form complexes of the macrocyclic ligand
5,7,7-trimethyl-1,4,8,11-tetra- azacyclotetradec-4-ene. For the nickel(II)
cation, singlet ground state, square planar, salts are formed with poorly
coordinating anions such as tetrachlorozincate, and triplet ground state, pseudoocta- hedral compounds with coordinating anions.
These occur as trans compounds (macrocycle in planar coordination) for the unidentate
anions NCS-, N3- and Cl-
and as cis compounds (macrocycle in folded coordination)for the chelating
anions acetylacetonate and oxalate. Different configurations of the chiral
nitrogen centres are optimum for planar and for folded coordination of the
macrocycle.
Infrared intensities as a quantitative measure of intramolecular interactions. XXXIX. Triaryl-phosphines, -phosphine oxides and -phosphine sulphides
Authors: Grindley TB , Johnson KF , Kaack H , Katritzky AR , Schiemenz GP , Topsom RD
Published: September 2010

The infrared intensities
for the v8 ring stretching band of series of meta- and
para-substituted triphenyl-phosphines, -phosphine oxides, and -phosphine
sulphides indicate the σ�R values: PPh2,-0.08; PPh2O,
+0.07; PPh2S, +0.06. All three groups show acceptor properties when
para to a strong donor substituent.
Reactions of 3,6-Diethoxyxanthen-9-one with alkylaluminium compounds
Authors: Evans JJ , Bagnell L , Eibl R , Holan G , Mole T
Published: September 2010

3,6-Diethoxyxanthen-9-one
reacts with trimethylaluminium to give 3,6- diethoxy-9-methylenexanthene
and a little 3,6-diethoxy-9,9- dimethylxanthene. In
similar reactions, triethylaluminium gives 3,6- diethoxy-9,9-diethylxanthene,
diisobutylaluminium hydride gives 3,6- diethoxyxanthene,
and tri-isobutylaluminium gives a mixture of 3,6- diethoxyxanthene
and 3,6-diethoxy-9-isobutylxanthene. The 3,6-diethoxy- 9-methylenexanthene has
been treated with base and chloroform or bromoform to obtain the corresponding
2,2-dihalo-3?,6?- diethoxyspiro[cyclopropane-1,9?-xanthene].
Infrared intensities as a quantitative measure of intramolecular interactions. XL. Di-para-substituted aryl phosphines
Authors: Kabachnik MI , Malakhov IG , Tsvetkov EN , Johnson KF , Katritzky AR , Sparrow AJ , Topsom RD
Published: September 2010

The infrared intensities
for the v8 ring stretching band of some meta- and para-substituted
phenyl-dialkylphosphines, -dichlorophosphines, and
-dialkoxyphosphines determine the σR values: PH2,
-0.05; PMe2, -0.08; PEt2, -0.08; PCl2, 0.07;
P(OEt)2, 0.06.
Nitration and bromination reactions of galbulin
Authors: McAlpine JB , Riggs NV
Published: September 2010

Nitration of the
1-phenyltetralin lignan, galbulin, occurs initially with dealkylative nitration
at C 9 and cleavage of the C 1-C 9 bond. Subsequent reaction of the carbonium
ion formed at C 1 with nitrate ion, and the degree of nitration of the aromatic
rings, determine the final products. In contrast, bromination is not dealkylative
and occurs initially at C 6? in ring c and subsequently at C 5 (ring A).
Bromination in acetic acid in the presence of pyridine is accompanied by an
unusual aromatic reaction, acetoxylation at C 8.
The hydrazinolysis of heterocyclic compounds. I. 1,4,6-Trimethylpyrimidine-2(1H)-thione and related compounds
Authors: Dickinson RG , Jacobsen NW , Gillis RG
Published: September 2010

The reaction of hydrazine
hydrate with 1,4,6-trimethylpyrimidine-2(1H)- thione is shown to follow two
major pathways. The first gives 4-amino- 5-hydrazino-1,2,4-triazole-3-thiol and
3,5-dimethyl-pyrazole. The second leads rapidly to 1-amino-4,6-dimethylpyrimidin-2(1H)-one
hydrazone, a bright red intermediate compound which is rapidly consumed
yielding 3,5-dimethylpyrazole and triaminoguanidine.
The N- aminopyrimidine structure assigned to the intermediate is discussed in
terms of its spectroscopic and chemical properties. Hydrazinolysis of
1,4,6-trimethylpyrimidin-2(1H)-imine similarly gives the same N- aminopyrimidine
as well as 2-methylamino-and 2-hydrazino-4,6- dimethylpyrimidine
from the Dimroth rearrangement. 1,4,6- Trimethylpyrimidin-2(1H)-one
gives only 3,5-dimethylpyrazole under the same conditions. Mechanisms of the
reactions are discussed.
Linear free energy relationship and some quantitative regularities of the of pressure on chemical reactions
Authors: El'yanov BS
Published: September 2010

A study has been made of
the applicability of a linear free energy relationship describing the effect of
pressure on the equilibrium and rate constants of chemical reactions. Some
properties of the relationship have been analysed and corollaries, including
linear dependences, obtained which make it possible to calculate reaction
enthalpies and entropies, volume changes and Hammett's p-constants at high
pressures. Ionization reactions have been used as examples to illustrate the
conclusions arrived at. The linear free energy relationship has been shown to
describe the effect of pressure up to 8000 bars on the ionization constants of
acids and on the pH of buffer solutions.
Studies in 4-Aminothiazolines. VII. Use of bromomalononitrile in the synthesis of 4-Aminothiazoline-5-carbonitriles and their subsequent hydrolysis byorthophosphoric acid
Authors: Singh A , Uppal AS
Published: September 2010

Bromomalononitrile on
condensation with N-substituted thioureas furnished 4-amino-3-aryl(or allyl)-2-imino-4-thiazoline-5-carbonitriles
(4). On acetylation in Ac2O/AcOH, (4) gave first mono acetyl
derivatives (5) and then diacetyl derivatives (6). Thiazolines (4) and acetyl
derivatives (5) underwent hydrolysis with orthophosphoric acid to the
corresponding amides (8) and (7) respectively.
The crystal and molecular stucture of μ-Bis(diphenylarsino)methanehexacarbonyldi-μ-chloro-dirhenium(I)-n-hexane (4/1)
Authors: Commons CJ , Hoskins BF
Published: September 2010

The crystal and molecular
structure of the n-hexane solvate of μ- bis(diphenylarsino)methane-hexacarbonyldi-μ-chloro-dirhenium(I), Re2(CO)6(Ph2AsCH2AsPh2)Cl2,
has been determined by three-dimensional X-ray diffraction methods. The complex
crystallizes in the space group Pī with a
15.763(1), b 19.077(1), c 12.233(1) Ǻ and α 88.745(10), β
110.506(5), γ 92.900(6)�. The structure was solved by conventional
Patterson and Fourier methods and refined by a block-diagonal least- squares
method to R and Rw of 0.045 and 0.054, respectively, for 7061
independent statistically significant reflections collected by counter methods.
The crystal consists of discrete molecules of the complex and n-hexane held
together by van der Waals
forces. There are two molecules of the dirhenium complex in the
crystallographic asymmetric unit with the n-hexane molecule situated about a
site of symmetry ī. The binuclear rhenium complex contains bridging
halogen atoms and a bridging diarsine ligand. Three carbonyl ligands are also
bonded to each rhenium atom, giving the metal atoms approximately octahedral
environments. The average Re-As, Re-Cl, and Re-C bond
lengths are 2.58, 2.52, and 1.89 Ǻ respectively.
Physicochemical studies on the aggregation of copper(II) and titanium(III) dialkyl phosphates
Authors: Cookson DJ , Wakefield RF , Smith TD , Pilbrow JR
Published: September 2010

Titanium(III) and copper(II)
salts of various dialkyl phosphoric acids have been prepared. Molecular weight
measurements on the copper(II) dialkyl phosphates show that they are monomeric
in ethanol but aggregate to dimeric forms in chloroform, and to trimeric and
tetrameric forms in dichloro- methane, while copper(II) di(2-
ethylhexyl) phosphate reaches a molecular weight
corresponding to a pentamer in n-hexane. Magnetic susceptibility measurements
indicate the absence of strong exchange coupling in the copper(II) dialkyl
phosphates. E.s.r. measurements have been made on the titanium(III) dialkyl
phosphates doped into the corresponding indium(III) dialkyl phosphates. Similar
measurements have been made on the copper(II) dialkyl phosphates doped into the
corresponding cadmium dialkyl phosphates. E.s.r. measurements have been carried
out on chloroform and dimethylformamide solutions of the copper(II) dialkyl
phosphates and the triplet state spectra observed at 77 K used to extract the
magnetic and structural parameters associated with the dimeric forms of the
copper(II) dialkyl phosphates. Infrared spectral measurements have been made on
the titanium(III), indium(III), copper(II) and cadmium(II) dialkyl phosphates
and the major peaks assigned.
Eight-coordinate complexes of titanium and niobium tetrachlorides with 1,8- Bisdimethylarsinonaphthalene
Authors: Kepert DL , Trigwell KR
Published: September 2010

Titanium and niobium
tetrachlorides form the eight-coordinate adducts [TiCl4(naars)2] and[NbCl4(naars)2] with 1,8-bisdimethylarsinonaphthalene.
The visible spectrum of the latter compound shows that as a result of the small
?bite? of this bidentate ligand, the order of orbital energies is dxy < dxz,
dyz < dx2-y2 < dz2.
Copper(I) complexes of 2-(Phenyliminomethyl)pyridine and some related ligands
Authors: Halbert EJ
Published: September 2010

A number of copper(I)
complexes of anils of pyridine-2-carbaldehyde with iodide and bromide as ions
have been prepared. The iodo compounds belong to the series [CuLI]2, thought to have a dimeric iodide-bridged
structure in the solid state. The compounds with bromide appear to have the
ion-pair structure [CuL2] [CuBr2]. The low solubility of
both types of complex in organic solvents severely limits their study.
Impurity effects on the apparent spin-spin relaxation times of 35Cl nuclear quadrupole resonance in some solid mixtures
Authors: Doolan KR , Hacobian S
Published: September 2010

Various monosubstituted and
disubstituted benzenes were mixed in varying amounts with p-dichlorobenzene to
form solid mixtures. The apparent spin-spin relaxation time, T*2,
of the 35Cl nuclear quadrupole resonance of each of these mixtures
was determined by a double pulsed super-regenerative oscillator (SRO) method
which has been described previously.1 The SRO was operated in the
logarithmic mode. The results show that electric quadrupole rather than
magnetic dipole interactions are mainly responsible for the broadening that was
observed for the 35Cl n.q.r. line of
p-dichlorobenzene due to the impurities. The results also indicate that the
para-disubstituted benzenes used formed uniform solid solutions with
p-dichlorobenzene over the concentration range studied.
N.I.R. absorption spectra of the phthalocyanines
Authors: Fielding PE , MacKay AG
Published: September 2010

Single crystal, film, and
selected vapour and solution n.i.r, absorption
spectra are reported for H2(pc), Cu(pc), Ni(pc), Zn(pc), Pd(pc),
Fe(pc), Mn(pc) and Cr(pc). The transitions have been
categorized and some suggestions are made concerning their origins.
The exchange of pyridine on Bis(β-alkanedionato)dipyridinenickel(II) complexes. A nitrogen-14 magnetic resonance study
Authors: Crea J , Lincoln SF
Published: September 2010

A 14N N.M.R.
study is reported of the exchange of pyridine (py) on
[Ni(bzac)2(py)2]
[k(298 K) = (4.6�0.5)x104 s-1, ΔH? = 38�3
kJ mol-1; ΔS? = -28�11 J K-1 mol-1],
[Ni(bzbz)2(py)2]
[k(298 K) = (2.7�0.3)x104 s-1; ΔH? = 38�3
kJ mol-1; ΔS? = -34�12 J K-1 mol-1],
[Ni(tfac)2(py)2]
[k(298 K) = (8.4�0.9)x103 s-1]; ΔH? = 32�3 kJ mol-1;
ΔS? = -58�11 J K-1 mol-1], and [Ni(hfac)2(py)2] [k(298 K)
< 2x103 s-1] in pyridine solution where the rate of pyridine
exchange = 2k[nickel(II) complex], bzac = 1- phenylbutane-1,3-dione;
bzbz = 1,3-diphenylpropane-1,3-dione; tfac = 1,1,1-trifluoropentane-2,4-dione; and hfac = 1,1,1,5,5,5- hexafluoropentane-2,4-dione. The
lability (298 K) of pyridine in the nickel(II) complexes is observed to
decrease as the electron withdrawing power, as assessed from appropriate Taft
parameters, of the β-alkanedionato ligand
increases.
A phenomenological theory of double injection with trapping
Authors: Bonham JS
Published: September 2010

A phenomenological theory
of double injection into an insulator with traps is derived under the injected
plasma approximation. Four probable trap configurations are considered:
discrete hole and electron traps, discrete hole and exponential electron traps,
exponential hole and discrete electron traps, and exponential hole and electron
traps. The traps are assumed to act as recombination centres. The large range
of possible j-V relations which emerges from these models is delineated. By
allowing the recombination radiation to cause photodetrapping the scaling law
(j/d) = f(V/d2) can be violated, explaining a common feature of
experimental work on anthracene. An exact calculation is used to confirm the
theory for a simple case.
The influence of polyelectrolytes on the thickening and filtration of hematite suspensions
Authors: Nicol SK , Wilson GR , Adamiak ZP
Published: September 2010

An experimental study of
the thickening and filtration characteristics of hematite suspensions consisting
of closely sized particles has been undertaken with a view to investigating the
influence of polyelectrolytes on these processes. The results show that a
certain optimal polymer addition exists for both processes after which no
further beneficial effects are observed. This polymer concentration is much
lower for filtration than for thickening. The origins of the maximum occurring
in the filtration rate with increasing polymer dosage is discussed in terms of
polymer adsorption. It is concluded from filtration experiments with coarse
de-slimed particles, and also a sintered disc, that the fall in filtration rate
at polymer concentrations above the optimum value occurs because of increasing
bed structure and not, as was formerly supposed, because of particle
restabilization.
Carbonyl halides of the Group VII transition metals. IV. Carbonyl halide complexes of rhenium(III)
Authors: Colton R , Garrard JE
Published: September 2010

The new halocarbonyl
complexes of rhenium(III), [Re(CO)2X4]- (X = Cl, Br), have been synthesized by the halogen oxidation of
[Re(CO)3X]4. On the basis of various physical
measurements a cis octahedral structure is proposed for these anions.
Benzo[c]cinnoline derivatives. VI. Reactions of halogenobenzo[c]cinnolines with potassium amide
Authors: Lewis GE , Prager RH , Ross RHM
Published: September 2010

The individual reactions of chloro- and iodo-benzo[cJcinnolines with potassium amide in ammonia
have been shown to yield mixtures of aminobenzo[c]cinnolines. The observed courses of reaction
are discussed in terms of mixed addition-elimination and elimination-addition mechanisms. A
small amount of tele-substitution (1,3-substitution) has been found to occur when 4-chlorobenzo[c]-
cinnoline reacts with potassium amide. Two possible mechanisms for this reaction are considered.
The use of p-Iodophenyl[125I] isothiocyanate for determination of N-terminal amino acids in nanomole quantities of protein
Authors: Burrell CJ , Cooper PD , Swan JM
Published: September 2010

Identification of the
N-terminal residue of 2.5-5 nmol of protein was
possible by means of a modified Edman reaction and p-iodophenyl[125I] isothiocyanate of high specific
activity. The second and third residues could also be identified. Yields of the
terminal residue were 25-50%, allowing approximate quantitation of the molar
content of protein. Use of the isotope allowed certain steps of the degradative
cycle to be examined in some detail, and preparation of this relatively non- volatile
labelled Edman reagent was safe, cheap and
convenient. ��� The synthesis and properties of the p-iodophenylthiohydantoins of 19 amino acids, and some side
products of the coupling reaction, are described.
Magnetic behaviour of some copper(II) nitrate complexes of benzimidazolylalkanols
Authors: Hamilton GJ , Kokot E
Published: September 2010

Complexes of the type CuL2(NO3)2(H2O)n
were prepared where L is benzimidazolylalkanol. When n
is 1 or 2, the magnetic behaviour follows the Curie-Weiss Law. On dehydration,
antiferromagnetism is observed.
The conformation of Mono- and Di-N-methyl trans-Decahydroquinazolines
Authors: Armarego WLF , Jones RAY , Katritzky AR , Read DM , Scattergood R
Published: September 2010

The conformational
equilibria of the title compounds all involve substantial contributions from conformers
with both lone pairs axial and with one pair axial and one equatorial.
The chlorination of Olean-12-enes
Authors: Bannon CD , Eade RA , Samaan HJ , Simes JJH
Published: September 2010

Chlorination of members of
the β-amyrin group of triterpenes by passing a mixture containing nitrosyl
chloride and chlorine into a solution of the triterpene in pyridine has yielded
the corresponding 12-chloro derivative. Members of the α-amyrin group did not
react under the conditions used. The N.M.R. and mass spectra of the
12-chloroolean-12- enes are discussed.
The structure of the compound previously designated 1,2,3-trihydroxynaphthalene (naphthopyrogallol)
Authors: Greenland H , Pinhey JT , Sternhell S
Published: September 2010

The compound previously
assigned the structure 1,2,3- trihydroxynaphthalene
has been shown on spectroscopic grounds to be
[1,1?-binaphthalenel-2,2?,3,3?,4,4?-hexol (1).
3,4,5,6,7,8-Hexahydronaphthalen-1(2H)-ones. Synthesis and photoaddition to (Z)-1,2-Dichloroethylene
Authors: Rae ID , Umbrasas BN
Published: September 2010

Several cyclohexanones have
been converted, via cyclohexylidenebutyric acids, into
3,4,5,6,7,8-hexa-hydronaphthalen-1(2H)-ones in good yield. Cyclododecanone
gives bicyclo[10,4,0]hexadec-1(12)-en-13-one. Heating 3,4,5,6,7,8-hexahydronaphthalen-1(2H)-one
with polyphosphoric acid gives 1,2,3,4-tetrahydronaphthalene, but the 7-methyl
octalone gives the 2- and 6-methyl tetralins. Photoreaction of (Z)-1,2- dichloroethylene
with 3,4,5,6,7,8-hexahydronaphthalen-1(2H)-one gives 11,12-dichlorotricyclo[4,4,2,0]dodecan-2-one.
The ethylene acetal of this adduct can be dechlorinated to give the acetal of
tricyclo[4,4,2,0]dec-11-en-2-one.
Photo- and electro-chemical processes at organic crystal electrodes. II. Oxidation of a solute in water by positive holes from an anthracene crystal
Authors: Lyons LE , McGregor KG
Published: September 2010

Although aqueous electrodes
have been used often to discharge positive holes emerging from an anthracene crystal, the mechanism has not yet been
elucidated in any one case. We have found that p-anilinobenzenesulphonate (1) prevents
all oxidation of the water, itself being oxidized with very nearly 100%
efficiency. To oxidize one negative ion, 1.99 � 0.01 holes are needed. The
product was N,N '-(1,1'-biquinone-4,4'-diimine)bisbenzene-p-suphonic
acid (2). An induction period before the production appeared in solution and
small deficiencies in the 100% oxidation were attributed to adsorption of a
monolayer (3.4 x 1013 ions cm-2) of the product ions on
the anthracene crystal, agreeing with an expected
area of 2.6 nm2 for an adsorbed ion. A 1 : 3 complex of iron(1) and
1,l0-phenanthroline gave similar results requiring one electron to oxidize a (+
2) positive ion with an adsorbed monolayer concentration of 7.3(�:0.1) x 1013
ions cm-1.
Activity models in the Na+,Zn2+/Cl-,SO42- reciprocal fused salt system
Authors: Anthony RG , Bloom H
Published: September 2010

The conformal ionic
solution model has been applied to the charge asymmetrical, reciprocal fused
salt system: Na+,Znz+/C1-,S042-.
This model takes into account binary and ternary type interactions as well as
the exchange equilibrium:

ZnCl2 + Na2SO4 ↔ ZnSO4
+ 2NaCl

Calculated ZnCl2 activities
are found to be in reasonable agreement with experimental values.
Donor-atom effects in the mass spectra of complexes of dipivaloylmethane and its monothio and dithio analogues
Authors: Macdonald CG , Martin RL , Masters AF
Published: September 2010

The progressive replacement
by sulphur in the isostructural planar nickel compounds bis(2,2,6,6-
tetramethylheptane-3,5-dionato)nickel(11) (1),
bis(2,2,6,6-tetramethyl-5-thioxoheptan-3-onato)nickel(11) (2) and
bis(2,2,6,6-tetramethylheptane-3,5-dithionato)nickel(11) (3) causes a change in
their positive electron impact mass spectra from one dominated by
metal-containing fragment ions (1) to one But 1 dominated by oxidized ligands
(3). Comparisons are also made with the spectra of tris(monothio-dipivaloylmethanato)cobalt(111)
and bis(1,l,1-trifluoro-4-thioxopentan-2-onato)nickel (11). Mass spectral peaks corresponding to mixed
ligand species were observed when mixtures of (1) and (2) were vaporized in the
mass spectrometer.
A study of conformation about the aryl C-N bonds in N-aryl imides by dynamic N.M.R. spectroscopy
Authors: Verma SM , Singh NB
Published: September 2010

A series of α, β-(9,10-dihydroanthracene-9,10-diyl)-N-arylsuccinimide
derivatives has been prepared and their N.M.R. spectral studies are reported.
The effect of the substituents at the N-phenyl
group on the conformational process about the aryl C-N bond has been
investigated.The asymmetric cage moiety
present in this system was employed for the conformational study.� The N.M.R. spectra provided evidence for the
non-planar conformation and restricted rotation about the aryl C-N bond in the
case of ortho-substituted
derivatives. Electronegative substituents were found to have a preferred
conformation (anti to the cage
moiety). The energy barrier (ΔGt) of the order of
86 kJ/mol has been determined by their temperature-dependent spectra. Free
rotation about the aryl C-N bond was observed for the meta- and para-substituted
derivatives. No buttressing effect by meta
substituents has been noticed.
The structure determination of a binuclear copper(II) complex of aTetra-Schiff base macrocycle
Authors: Hoskins BF , McLeod NJ , Schaap HA
Published: September 2010

The structure of the
complex Lcu2Cl2,6H2O (where LH2 is
the tetra-Schiff base macrocycle formed as the
condensation product of propane-1,3-diamine and 2-hydroxy-5-methylisophthal-
aldehyde in the mole ratio 2: 2) was determined by single-crystal X-ray diffraction
methods. The crystals are monoclinic, a
7.720(1), b 17.079(1), c 11.171(1) � and β 91.50(1)�, with
two molecules per unit cell. It has proved difficult to resolve the ambiguity
between the three possible space groups (C2, Cm, and C2/m) and the
initial model has been refined in each using a full-matrix least-squares
method. The space group C2/m seems
the most likely and the structure is described in it; R 0.049 for the 1369
independent reflections measured using counter methods. The structure analysis
has confirmed the anticipated cyclic structure of the ligand with the two
copper atoms held together in a binuclear arrangement by the planar N4O2
donor set; the Cu.. .Cu distance is 3.133(1)�. Each copper atom has a distorted
square-pyramidal environment with the apical position of each being occupied by
a chlorine atom; the two chlorine atoms are on the opposite sides of the macrocycle. The water molecules are not coordinated, but
form an extensive system of hydrogen bonding throughout the crystal with discrete
binuclear molecules of the LCu2Cl2 complex.
Crystal structure of Bis(N,N-diisobutyldithiocarbamato)nickel(II)
Authors: Raston CL , White AH
Published: September 2010

The crystal structure of
the title compound, [Ni(S2CNBu12)2],
has been determined by X-ray diffraction at 295 K and refined by least squares
to a residual of 0.058 for 2031 'observed' reflections. Crystals are
monoclinic, P21/a, a =
16.705(6), b = 13.062(5), c = ll.799(5) �, β = 97.03(3)�, Z =
4. The nickel atom is chelated in an approximately square planar array by two symmetric
bidentate dithiocarbarnate ligands, <Ni-S) 2.201
�. The ligand symmetry is a good approximation to C2; there is a
strong interaction between the tertiary hydrogen atoms and nearby sulphur and nickel atoms.
Preparation and characterization of the double acetates of zinc, cadmium and mercury(II)
Authors: Malhotra KC , Katoch DS
Published: September 2010

Double acetates of
composition M2[M(OAC)4]3xAc2O,
where x may have a value of four or six, have been isolated from acetic
anhydride by mixing the anhydrous acetates of zinc, cadmium and mercury and the
acetates of alkali metals, ammonium and thallium in acetic anhydride. From the
conductance, molecular weight, 1.r. and t.g.a. studies, their structures have
been elucidated.
Basic halides and related species of molybdenum(III). II. Spectroscopic and magnetic properties of MoOF(H2O)3 and MoOCl(H2O)3
Authors: Stabb DJ
Published: September 2010

Two basic halides of
molybdenum(111), namely MoOF(H2O)3 and
MoOCl(H2O)3 (some samples
containing additional loosely bound water), were investigated by absorption
spectroscopy in the range 200-50000 cm-1, and by magnetic
susceptibility measurements over a temperature range of 100-300 K. Infrared
spectra showed bands at about 670 and 1600 cm-l, but not in the
range 800-1100 cm-1. Electronic spectra showed poorly defined bands
superimposed on strong general absorption. Very weak paramagnetism
was observed: this was field dependent. The results are interpreted to show the
compounds to be oxygen-bridged polymers [MOX(H2O)3O]n,
rather than species containing Mo=O or Mo-0-H groups.
Insecticides. VI. Crystal structure of methoxychlor [1,1,1-Trichloro-2,2-bis(p-methoxyphenyl)ethane]
Authors: Smith G , Kennard CHL , White AH
Published: September 2010

The crystal structure of methoxychlor was determined by the symbolic addition
procedure from three-dimensional diffractometer data with 1507 reflections. The
unit cell is triclinic, a =
1221.4(4), b = 1069.2(3), c = 636.2(2) pm; α ( = 100.60(2)�, β
= 84.49(2)� and γ = 98.26(2)� with Z = 2. Least-squares refinement reduced
the residual R to 0.048. Molecular dimensions are of the same order as those
found in p,p'-DDT except that the angle between the normals to the benzene planes (77.7 �) is greater than in p,p?-DDT (64.9�).
Depsidone synthesis. V. The chemistry of psoromic acid: a reinvestigation
Authors: Huneck S , Sargent MV
Published: September 2010

The structure of the lichen
depsidone psoromic acid (1)
(4-formyl-3-hydroxy-8-methoxy-1,9-dimethyl-ll-oxo-11H-dibenzo[b,e][l,4]dioxepin-6-carboxylic acid) is confirmed by a
combination of spectroscopic, degradative and synthetic experiments. Smiles
rearrangements encountered in the degradation of psoromic
acid are discussed.
Synthesis of orcinol tridepsides and aphthosin, an orcinol tetradepside
Authors: Bryan AJ , Elix JA , Norfolk S
Published: September 2010

Total syntheses of the
lichen depsides, gyrophoric
acid, methyl gyrophorate, 4-O-methylgyrophoric acid, tenuiorin, umbilicaric acid, hiascic acid
and aphthosin are described.
Methylation of tricarbonylcyclohexadienyliron salts with lithium dimethylcuprate
Authors: Pearson AJ
Published: September 2010

The reaction between
various tricarbonylcyclohexadienyliron salts and
lithium dimethylcuprate leads to stereospecific, regioselective methylation. Deuterium-labelled compounds
are used to establish that alkylation occurs at the face of the dienyl system
opposite to that occupied by Fe(CO)3.
Mass spectral study of the vapour of aluminium 2,2',2'-nitrilotriethoxide
Authors: Lacey MJ , Macdonald CG
Published: September 2010

The mass spectrum of
aluminium 2,2',2-nitrilotriethoxide is consistent with a dimeric structure for
the compound in the gas phase.
Photolysis of 4,5-Epoxycholest-2-enes
Authors: Coxon JM , Hii GSC
Published: September 2010

Photolysis of 4α5-epoxy-5α
- and 4β,5-epoxy-5β -cholest-2-enes in acetone (30004-�. lamps)
effects molecular rearrangement to A-nor-B-homo-5β- and -5α -cholest-2-en-6-ones
respectively.
Bonding in d10 transition metal complexes. IV. Infrared, Raman and N.Q.R. studies of some dihaloaurate(I) complexes
Authors: Bowmaker GA , Whiting R
Published: September 2010

The infrared and Raman
spectra of bis(N,N-dibutyldithiocarbamato)gold(111)
dichloroaurate(1), [(Bu2NCS2)2AU] AuCl2,
and the corresponding bromo and iodo compounds have been measured, and the
anion vibrational frequencies assigned. The results are compared with those for
other MX2- ions (M = Cu, Ag; X = C1, Br, I). The chlorine n.q.r.
frequencies for the above-named compound, and the corresponding
tetraalkylammonium salts, [R4N] AuCl2 (R = Et, Bu), have
also been measured. A Townes and Dailey analysis of the results indicates an
ionic character of about 68% for the Au-Cl bond in the AuCl2- ion,
and a net charge of about + 0.36e on the Au atom. These results are compared
with those for some related metal halide complexes.
Thermodynamics of metal-ligand bond formation. XXII. Zinc(II) and cadmium(II) dialkyldithiocarbamates
Authors: Ang L , Graddon DP
Published: September 2010

Thermodynamic data are
reported for dimerization of dialkyldithiocarbamates,
(R2NCS2)2Cd, and for addition of heterocyclic
bases to (R2NCS2)2Cd and (R2NCS2)2Zn
in benzene solution. Enthalpies of reaction are comparable to those of
corresponding dithiophosphates, but adduct formation and dimerization constants
are smaller and the dithiocarbamates add only one
molecule of base. Though probably bidentate, 2,2'-bipyridine forms less stable
adducts with (R2NCS2)2Zn than does pyridine.
Pseudohypericin and other phenanthroperylene quinones
Authors: Cameron DW , Raverty WD
Published: September 2010

The recently revised
structure (4) proposed for pseudohypericin has been confirmed by spectroscopic data
and two independent syntheses. The phenanthroperylene quinones (7) and (a), the
former corresponding to fringelite F, have been synthesized from the corresponding
anthrones (16) and (17).A revised structure for
cyclopseudohypericin (5) has been established on the basis of spectroscopic evidence.
Other reactions of pseudohypericin are discussed.
The formation of O,O-isopropylidene derivatives from 16-hydroxyoleanenes
Authors: Hensens OD , Khong PW , Lewis KG
Published: September 2010

Re-examination of the reactions of primulagenin
A, longispinogenin
and chichipegenin with acetone has shown that isopropylidene derivatives may be obtained in all cases.
With chichipegenin two of the three possible isomeric
isopropylidene derivatives were isolated. The effect
of alteration of the conformation of ring v by the introduction of a Δ13(18) double bond on
the ease of formation of the 1,3-dioxan ring has been examined in the case of
the 3β,16α,28-triol system.
The chemistry of pyrrolic compounds. XXXII. Synthesis of isocoproporphyrin tetramethyl ester and related compounds
Authors: Clezy PS , Hai TT
Published: September 2010

The acetylporphyrin (la)
has been prepared by the oxidative cyclization of an intermediate bilene-b salt. By standard procedures this
porphyrin has been converted into the ethyl (lb) (isocoproporphyrin tetramethyl
ester), vinyl (lc), hydroxyethyl (1d) and deacetyl (1e) derivatives. These
compounds have been reported to occur in the faeces of animals suffering from
certain porphyric conditions.
Studies in the chemistry of polyhalogenobenzene compounds. The synthesis and reactivity of 2,3,5,6- and 2,3,4,5-tetrachlorobenzenesulphonyl chlorides and related compounds
Authors: Chivers GE , Cremlyn RJW , Cronjie TN , Martin RA
Published: September 2010

2,3,5,6-Tetrachlorobenzenesulphonyl
chloride (2) and pentachlorobenzenesulphonyl chloride (4) have been obtained
from the corresponding sulphonic acids (3) and (5) by treatment with phosphorus
pentachloride. The sulphonyl chlorides have been characterized as a series of
polychlorobenzene- sulphonamides, some of which have been converted into
N-trichloromethylsulphenyl derivatives. The reaction of 1,2,4,5-tetrachlorobenzene
with chlorosulphonic acid has been reinvestigated; comparatively short reaction
periods gave mainly bis(pentachloropheny1) sulphide, and prolonged heating
afforded hexachlorobenzene. Possible routes to these products are briefly
discussed. Attempts to obtain 2,3,5,6-tetrachlorobenzenesulphonohydrazide (10)
were unsuccessful; but the corresponding sulphonyl azide (11) has been prepared
and its reactions with triphenylphosphine, norbornene and cyclohexene
investigated.
13C N.M.R spectra of quinoline and methylquinolines. The magnitude of the vicinal (peri) 3JCCCH coupling constants
Authors: Johns SR , Willing RI
Published: September 2010

The 13C chemical
shifts and the 13C-1H coupling constants of quinoline, isoquinoline and five methylquinolines are reported. A vicinal (peri) 3JCCCH
coupling constant of approximately 5 Hz is observed between both C5-H4 and
C4-H5. The α-, meta- and para-methyl substituent shifts are similar in
magnitude to those observed for methylbenzenes and methylpyridines
but the ortho-shifts vary in both
sign and magnitude.
Synthesis of 2-Aryl-4-arylazo-2-thiazolin-5-ones and their reaction with aromatic amines
Authors: Khalil AM , El-Gawad IIA , Hassan HM
Published: September 2010

2-Aryl-4-arylazo-2-thiazolin-5-ones
are prepared by a coupling reaction between thioaroylglycine
and the appropriate diazonium salt. Their
heterocyclic ring is readily opened by the action of primary aromatic amines in
acetic acid containing a catalytic amount of sodium acetate with the formation
of 1,5,Nx-triaryl-1H-l,2,4-triazole-3-carboxamides.
Gas-phase decompositions of 1,1-dimethoxyethane and 1,1-diethoxyethane catalysed by hydrogen chloride
Authors: Drager M , Failes RL
Published: September 2010

The
hydrogen-chloride-catalysed, gas-phase decompositions of 1,l-dimethoxyethane
and 1,l-diethoxy- ethane to alkyl vinyl ethers and an alcohol have been studied
over the temperature ranges 254-322 and 225-285�C, respectively. The reactions
are first order in each reactant and the second-order rate constants are given
by

K2 = 1013.14exp(-112000/RT) for 1,l-dimethoxyethane

and

k2 = 1012.66exp(-96200/RT) for 1,l-diethoxyethane

with k2 in s-l
ml mol-1 and R in J K-1
mol-1. Substituent effects and the relative effectiveness of
hydrogen chloride and hydrogen bromide as catalysts are consistent with those
described previously for HX-catalysed alcohol and ether decompositions.
Carbon-13 nuclear magnetic resonance spectroscopic study of tricarbonyldieneiron complexes: methyl substituent effects
Authors: Pearson AJ
Published: September 2010

From a comparison of β-effects
given by methyl substituents in tricarbonyldieneiron
complexes with those of the corresponding uncomplexed
1,3-dienes, it is concluded that bonding to iron results in a change in p-bond orders of the ligand. This change is consistent
with the structure (1) making an important contribution to bonding in these
complexes.
Proton N.M.R. spectra of 1-substituted benzocyclobutenes (Bicyclo[4,2,0]octa-1,3,5-trienes)
Authors: Bubb WA , Sternhell S
Published: September 2010

The p.m.r. spectra of 15
1-substituted benzocyclobutenes (bicyclo[4,2,0]octa-1,3,5-trienes) were
analysed. The effect of substituents on the N.M.R. parameters is discussed and
compared with analogous effects in other systems, especially acenaphthene which
is considered a relevant model. It is concluded that substituent effects in
1-substituted benzocyclobutenes are in no way exceptional, but they appear to
be less quantitatively additive than in the acenaphthene system.
The chemistry of the Euphorbiaceae. XXIV. Lup-20(29)-ene-3β,16β,28-triol from Beyeria brevifolia var. brevifolia
Authors: Errington SG , Ghisalberti EL , Jefferies PR
Published: September 2010

A new triterpene triol from the title plant has been shown to be
lup-20(29)-ene-38,168,28-trio1 (1) by degradation to deoxyallobetulin
(7) and to lupane-3β,16β-diol (4). Treatment of the triol (1) with subsequent acetylation,
and of betulin (10) with concentrated hydrochloric
acid in ethanol was found to give the 20,28-epoxy-19αH-lupane derivatives
(12) and (13) respectively. Amendments are given to the names of a number of
plants examined in this series.
The electron affinity of tetracyanoethylene and other organic electron acceptors
Authors: Lyons LE , Palmer LD
Published: September 2010

Information on the
molecular structure of tetracyanoethylene and its mononegative ion is used to
derive the electron affinity of tetracyanoethylene from the experimentally
determined threshold energy for photodetachment of electrons from the negative
ions. The resultant electron affinity of 2.3(� 0.3) eV is 0.6(� 0.4) eV less
than a value derived by the magnetron surface ionization technique. Relative
electron affinities for the strong electron acceptor organic molecules, which
are known from charge-transfer spectra, are placed on an absolute scale using
the photodetachment result for tetracyanoethylene.
Solution chemistry in dichloroacetic acid. II. Conductance studies of acids and bases in dichloroacetic acid
Authors: Malhotra KC , Sud RG
Published: September 2010

Conductance measurements of
protonic acids and Lewis acids have been carried out
in dichloroacetic acid at 25 � 0.l�C. Λ0,
values have been determined for these acids; it is found that there is extensive
ion-pair formation in solution. The role of CHCl2CO2H as
a differentiating solvent has been explored. Triple-ion formation for SbCl5
and AlBr3 is indicated which is supported by log C against logΛc curves. Similar trends have been
indicated for organic tertiary bases in dichloroaceticacid. Conductometric
studies of the same salts in dichloroacetic acid have
also been carried out. Fluorosulphuric acid has been developed as an acidic titrant for the estimation of bases in dichloroacetic
acid.
A stereospecific route to (Z) and (E) β-alkyl bromoalkenes
Authors: Gregson RP , Mirrington RN
Published: September 2010

A stereospecific route to
(Z)- and (E)-1-bromo-3-methylbut-1-ene (1) and (2) is described. Some previous
work has been clarified.
Sporidesmins. XV, The 13C nuclear magnetic resonance spectra of sporidesmin and sporidesmin-D. The evidence in the spectra for strain imposed by an epidithio bridge
Authors: Ronaldson JW
Published: September 2010

The proton-noise-decoupled 13C
N.M.R. spectra of sporidesmin and sporidesmin-D
are presented. The detailed assignments were worked out from the undecoupled spectrum of sporidesmin-D.
The 3-methyl resonance moved downfield (by 7.3 ppm) upon cleavage of the -S-S-
bridge in sporidesmin while the peaks of the two
quaternary carbons to which the sulphurs are bound
moved upfield (by 4.7 ppm). Lactam N-methyl and indoline
N-methyl proton resonance decoupling showed that their p.m.r.
assignments should be reversed. The electro-negativity of nitrogen, sulphur and
carbonyl groups increased the coupling constants of the 3-CH3 by 7Hz
and of the 11-CH by 10 Hz. The carbon of the lactam N-methyl was shielded by 14
ppm. There were six three-bond couplings, four HCN13C and two HCO13C,
evident but no non-aromatic HCC13C couplings.
A convenient new Method for the preparation of vanadium(III) β-diketonates
Authors: Dilli S , Patsalides E
Published: September 2010

The vanadium(111) tris-β-diketonates derived from pentane-2,4-dione and 13 other β-diketones
were prepared by reduction of oxovanadium(1V) sulphate with sodium dithionite and chelation of the
vanadium(111) with ligand in an aqueous alcohol medium. The chelate prepared
with pentane-2,4-dione was also obtained
by reduction of ammonium vanadate and oxobis(pentane-2,4-dionato)-vanadium(1V). Preparative
details are given and the advantages, and some difficulties, of the method are
discussed.
Central nervous system active compounds. II. The synthesis of some 4-, 5-, 6- and 7-substituted caprolactams
Authors: Duong T , Prager RH , Tippett JM , Ward AD , Kerr DIB
Published: September 2010

The synthesis of
caprolactam derivatives substituted at C4, C5, C6 and C7 with alkyl, aryl, acyl
and hetero substituents is described. A variety of synthetic approaches to
these compounds have been investigated and assessed, particularly for the
synthesis of C4- and C6-substituted compounds. A significant number of the C4-,
C6- and C7- substituted compounds prepared show central nervous system
activity, ranging from convulsants to depressants depending on the position and
nature of the substituent group.