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Showing papers by "D. Bryan Sowerby published in 1992"


Journal ArticleDOI
TL;DR: The diphenylantimony(III)phosphorodithioates, Ph 2 SbS 2 P(OR) 2 where R = Me, Et, i Pr and Ph, have been prepared and the methyl and isopropyl derivatives obtained as crystalline solids as mentioned in this paper.

48 citations


Journal ArticleDOI
TL;DR: The crystal structures of the complex [Me 4 Sb] 2 [MeSbI 4 ] (1) and its precursors MeSb 2 (2 ) and [Me SbI]I (3 ) are reported in this paper, where they associate via iodine bridges to form linear chains with alternating short and long Sb-I distances.

33 citations


Journal ArticleDOI
TL;DR: In this article, the course of the reaction between triphenylantimony dichloride and silver oxalate depends on both the solvent and temperature at which the reaction is carried out.
Abstract: The course of the reaction between triphenylantimony dichloride and silver oxalate depends on both the solvent and temperature at which the reaction is carried out. No reaction occurs in toluene at room temperature, but on refluxing the solution, crystals of [SbPh4][SbPh2(ox)2]1[ox = oxalate(2–)], an ionic form of SbPh3(ox), are obtained. Covalent SbPh3(ox), on the other hand, is probably the initial product of reaction in methanol at room temperature, but on recrystallisation from hot methanol, crystals of a methoxy derivative, [SbPh3(OMe)]2ox 2, are obtained. Structures have been determined for both compounds. Compound 1 consists of tetrahedral [SbPh4]+ cations and octahedral [SbPh2(ox)2]– anions containing two chelating oxalate groups and phenyl groups in cis positions. The methoxy derivative 2 is centrosymmetric, with a quadridentate oxalate group and each antimony octahedrally co-ordinated to three phenyl groups, one methoxy group and two oxygens from the oxalate group. A quadridentate oxalate group is also present in (SbPh4)2ox 3, obtained from [SbPh4]Br and silver oxalate. The structure contains two essentially identical, independent, centrosymmetric molecules with antimony again in distorted-octahedral co-ordination.

28 citations


Journal ArticleDOI
TL;DR: In this article, the structure of the first compound has been confirmed by X-ray diffraction as a fluorine-bridged diantimony compound, where the antimony atoms are, respectively, in trigonal-bipyramidal and distorted-octahedral coordination.
Abstract: Oxidation of diphenylantimony fluoride with chlorine leads to diphenylantimony trichloride as the only isolable product, while the corresponding reaction with bromine gives, in addition to SbPh2Br3, the bromide fluorides, Sb2Ph4Br5F, SbPh2Br2F, Sb2Ph4Br3F3 and SbPh2BrF2. The structure of the first compound has been confirmed by X-ray diffraction as a fluorine-bridged diantimony compound, SbPh2Br2F·SbPh2Br3, where the antimony atoms are, respectively, in trigonal-bipyramidal and distorted-octahedral co-ordination. Hydrolysis during attempts to obtain crystals of the second compound produced the oxygen-bridged (SbPh2BrF)2O, which contains a strong intramolecular fluorine bridge, again giving antimony atoms in both trigonal-bipyramidal and octahedral co-ordination. As an alternative approach to the preparation of mixed chloride fluorides, reactions between diphenylantimony trichloride and KF, AgF and arsenic trifluoride were investigated. There was no reaction with the first two reagents but the product with arsenic trifluoride was a disordered mixed halide, shown by X-ray crystallography to be SbPh3Cl1.8F0.2.

6 citations


Journal ArticleDOI
TL;DR: In this paper, the authors showed that diphenylantimony fluoride and thiocyanate with t-butyl hydroperoxide leads to tetrameric products containing a four-membered Sb2O2 ring with a further antimony atom attached via a single oxygen bridge to each of the ring antimony atoms.
Abstract: Oxidation of diphenylantimony fluoride and thiocyanate with t-butyl hydroperoxide leads to tetrameric products containing a four-membered Sb2O2 ring with a further antimony atom, carrying respectively either two fluorine or two thiocyanate substituents, attached via a single oxygen bridge to each of the ring antimony atoms This is in contrast to the formation of simple four-membered ring compounds when the corresponding bromide and chloride are oxidised The reaction between [Ph2SbOBr]2 and silver oxalate is not a simple substitution and the product is a complex salt whose cation contains a planar twelve-membered Sb6O6 ring

4 citations