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

DOI: 10.1039/dt9960004471

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 4471 - 4478 (1996)

Update date:2022-08-03

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Authors:

Dann, Sandra E.Dann, Sandra E.

Genge, Anthony R. J.Genge, Anthony R. J.

Levason, WilliamLevason, William

Reid, GillianReid, Gillian

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Article abstract of DOI:10.1039/dt9960004471

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.

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Product name:[SnCl4(C6H5S(CH2)3SC6H5)]

Cas No:185853-72-9

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