- Tri- and di-arylantimony( V) thiocyanates and mixed halide thiocyanates; crystal structure of triphenylantimony( V) di-isothiocyanate
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A series of triarylantimony(V) dithiocyanates has been prepared by oxidising the appropriate antimony(III) compound with thiocyanogen. IR and 14N NMR spectroscopy indicate the presence of terminally N-bonded thiocyanate groups and this has been confirmed by a crystal structure determination for the SbPh3(NCS)2. The asymmetric unit contains three independent trigonal bipyramidal molecules, which differ in the orientations of the axial N-bonded thiocyanates and the phenyl groups in the equatorial plane, and there may be weak C-H ... S interactions. Treatment of SbPh2X3, where X = Br or Cl, with KSCN gave K[SbPh2(NCS)4] and attempts to prepare SbPh2(NCS)3 and related diphenylantimony(V) mixed halide thiocyanates, SbPh2Xn(NCS)3 - n where X = Br or Cl and n = 0-2, by treating appropriate diphenylantimony(III) precursors with thiocyanogen or thiocyanogen bromide or chloride gave products which in many cases underwent reorganisation during recrystallisation. Samples of SbPh2(NCS)3, SbPh2Br(NCS)2, SbPh2Br2(NCS) and SbPh2Cl2(NCS), and SbPh3Br(NCS) have, however, been isolated as microcrystalline solids.
- Forster, Glynis E.,Begley, Michael J.,Sowerby, D. Bryan
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p. 263 - 274
(2007/10/03)
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- Diphenylantimony(V) Oxide Halides and Thiocyanate; the Crystal Structures of Dimeric Diphenylantimony(V) Bromide Oxide and Tetrameric Diphenylantimony(V) Oxide Fluoride and Thiocyanate
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Dimers containing a four-membered Sb2O2 ring with antimony atoms in distorted trigonal-bipyramidal co-ordination were obtained when either diphenylantimony(III) chloride or bromide was oxidised with tert-butyl hydroperoxide; the crystal structure of SbPh
- Southerington, I. Gary,Forster, Glynis E.,Begley, Michael J.,Sowerby, D. Bryan
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p. 1995 - 2004
(2007/10/02)
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- Phenylantimony(V) Fluoride Halides: Isolation and Crystal Structures of SbPh2Br2F*SbPh2Br3, (SbPh2BrF)2O and SbPh3Cl1.8F0.2
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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 coordination.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.
- Bone, Stephen P.,Begley, Michael J.,Sowerby, D. Bryan
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p. 2085 - 2092
(2007/10/02)
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- Lewis acidity of Ph2SbX3, where X=Cl or Br. Crystal structures of Ph2SbCl3*H2O and Ph2SbBr3*MeCN
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Diphenylantimony trichloride and tribromide are weak Lewis acids forming 1/1 addition compounds with acetonitrile which rapidly lose coordinated nitrile at room temperature.The structure of Ph2SbBr3*MeCN has been determined; the acetonitrile, antimony, an
- Bamgboye, T. Tunde,Begley, Michael J.,Sowerby, D. Bryan
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