- Symmetry of the co-ordination sphere of di-n-butyltin(IV) in complexes with sulfanylcarboxylic acids
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Four di-n-butyltin(IV) complexes have been prepared with sulfanylacetic, 2-sulfanylpropionic, sulfanylsuccinic and 2,3-disulfanylsuccinic acid, using two different procedures. The compounds were characterised by elemental analysis, Fourier-transform, Raman, 119Sn Moessbauer, 1H, 13C and 119Sn NMR spectroscopy. The IR and Raman data indicate the presence of bidentate carboxylate groups, non-linear C-Sn-C bonds, and Sn-S bonds. The results of Moessbauer spectroscopic measurements, based on point-charge model calculations, have shown the general occurrence of trigonal-bipyramidal environments at tin(IV). The multinuclear NMR studies also suggested the {O,S} co-ordination of the di-n-butyltin(IV) fragment, within the cyclic oligomeric complexes.
- Gajda-Schrantz, Krisztina,Nagy, Laszlo,Kuzmann, Erno,Vertes, Attila,Holecek, Jan,Lycka, Antonin
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p. 2201 - 2205
(2007/10/03)
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- Preparation and characterization of triorganotin(IV) derivatives of mercaptocarboxylic acids. Crystal structure of
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The syntheses and tin-119m Moessbauer spectroscopic data are reported for the tri-n-butyl, tricyclohexyl- and triphenyltin(IV) derivatives of mercaptoacetic and 2-mercaptobenzoic acids.A four-coordinate tetrahedral geometry at tin is assigned for (cyclo-C6H11)3SnSCH2C(O)OH and for the (C6H5)3SnSCH2C(O)O- and (C6H5)3SnSC6H4C(O)O- anions, isolated as the dicyclohexylammonium and iso-S-benzylthiuronium salts, respectively.The sulfidotin in R3SnSCH2C(O)OSnR3 and R3SnSC6H4C(O)OSnR3 is also four-coordinate, but the carboxylatotin is four-coordinate for R=C6H5 and five-coordinate for R=n-C4H9.The Moessbauer quadropole splitting in the butyltin case indicates a trans-C3SnO2 trigonal bipyramidal configuration.The coordination assignment for the two tin atoms in bis(triphenyltin)-2-mercaptobenzoate is confirmed by X-ray crystallography.The compound crystallizes in space group P21/c with a 14.293(4), b 17.456(2), c 15.624(1) Angstroem, β 107.40(1) deg; Z=4.The structure was refined to an R factor of 0.035 for 5837 observed reflections.The carbonyl oxygen of the molecule is positioned roughly halfway between the carboxylatotin (Sn***O 2.765(3) Angstroem) and sulfidotin (Sn***S 3.016(1) Angstroem), distorting somewhat the tetrahedral geometries at both tin sites.
- Ng, Seik Weng,Chin, Kwai Lan,Wei, Chen,Das, V. G. Kumar,Mak, Thomas C. W.
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p. 207 - 214
(2007/10/02)
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