Issue 23, 1996

Synthesis, solution and magic angle spinning tin-119 nuclear magnetic resonance studies and crystal structures of dithioether complexes of tin(IV) halides

Abstract

The compounds SnX4 reacted with 1 molar equivalent of dithioether, L–L, in dry CHCl3 solution to give the six-co-ordinate species [SnX4(L–L)][X = Cl, L–L = MeS(CH2)nSMe, o-C6H4(SMe)2 or PhS(CH2)nSPh (n= 2 or 3); X = Br, L–L = MeS(CH2)nSMe or o-C6H4(SMe)2] in high yield as white or pale yellow powdered solids. Using SnBr4 and PhS(CH2)nSPh or SnI4 with MeS(CH2)nSMe did not produce isolable products, although solution 119Sn-{1H} NMR spectroscopy provided evidence for their existence at low temperatures. X-Ray structural studies on [SnCl4{MeS(CH2)2SMe}], [SnCl4{MeS(CH2)3SMe}], [SnCl4{o-C6H4(SMe)2}], [SnCl4{PhS(CH2)3SPh}] and [SnBr4{MeS(CH2)3SMe}] confirmed an S2X4 donor set with the dithioether acting as a bidentate chelate. Variable-temperature solution 1H and 119Sn-{1H} NMR spectroscopic studies showed that the complexes are extremely labile and ligand dissociation and pyramidal inversion are fast except at low temperatures. Magic angle spinning 119Sn NMR data for [SnCl4(L–L)] are reported. The crystal structure of cis-[SnI4{MeS(O)(CH2)3SMe}2], obtained as a decomposition product from the SnI4–MeS(CH2)3SMe reaction, shows monodentate sulfoxide (O) co-ordination.

Article information

Article type
Paper

J. Chem. Soc., Dalton Trans., 1996, 4471-4478

Synthesis, solution and magic angle spinning tin-119 nuclear magnetic resonance studies and crystal structures of dithioether complexes of tin(IV) halides

S. E. Dann, A. R. J. Genge, W. Levason and G. Reid, J. Chem. Soc., Dalton Trans., 1996, 4471 DOI: 10.1039/DT9960004471

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