Preparation, vibrational spectra and crystal structure of tris(trimethyltin) tetrathiophosphate (Me3SnS)3PS

doi:10.1016/S0022-328X(00)99455-5

Journal of Organometallic Chemistry

Volume 342, Issue 2, 15 March 1988, Pages 177-183

https://doi.org/10.1016/S0022-328X(00)99455-5 Get rights and content

Abstract

Tris(trimethyltin) tetrathiophosphate (Me₃SnS)₃PS has been prepared by the reaction of (Me₃Sn)₂S with PSCl₃. Its IR and Raman spectra are reported and discussed, and ³¹P NMR spectral data presented. A X-ray diffraction study shows that crystals of (Me₃SnS)₃PS consist of discrete monomeric molecules in which both the tin and phosphorus atoms are four-coordinate and the Me₃Sn groups are covalently bonded to the sulphur.

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Cited by (12)

Conformations and coordination properties of trialkyltrithiophosphites in copper(I) complexes
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Citation Excerpt :
As it was pointed out above, most “free” trialkyltrithiophosphites and triphenyltrithiophosphite in the crystalline phase have a propeller gauche, gauche, gauche-conformation [16–19] and a mixture of conformers with gauche- and trans orientation of the alkylthio-groups with respect to the phosphorus lone electron pair in the gaseous [12] and liquid phases and in solutions [10,11]. No drastic conformational changes are observed in four-coordinated phosphorus compounds: in thiophosphoryl derivatives [20,21] the same orientations with respect to double bonds are most favorable. Upon the complex formation trithiophosphites undergo significant conformational changes if we consider the orientation of alkyl and arylthio-groups with respect to the phosphorus–metal bond.
A series of complexes (RS)₃P·CuBr with R=Et, Pr, Bu, i-Pr as well as the complex of (PrS)₃P·CuSCN were studied by X-ray single-crystal diffraction. Coordination properties of thiophosphites were found to be essentially different from their oxygen and nitrogen analogues and depend on the nature of the metal center, substituents at sulfur atoms, the conditions of reactions and of the crystal growth. All trithiophosphites in the studied copper(I) complexes except the isopropyl derivative exhibit bidentate coordination with both phosphorus and sulfur participating in coordination bonds with copper.
Trithiophosphites increase their conformational multiformity upon complexation regardless of the coordination mode, propyl and butyl derivatives being conformationally inhomogeneous in crystals. Unusual cis-conformations about the P–S bond, which are not observed for “free” trialkyltrithiophosphites or their phosphoryl and thiophosphoryl analogues, are realized in the complexes.
The complexation results in the significant high-frequency shift of the symmetric and asymmetric PS₃ stretching vibrations in the Raman spectra of complexes regardless of the coordination mode and in minor changes of the C–S stretching vibrations in comparison with the spectra of the “free” ligands.
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Preparation, vibrational spectra and crystal structure of tris(trimethyltin) tetrathiophosphate (Me3SnS)3PS

Abstract

J. Organomet. Chem.

J. Organomet. Chem.

J. Organomet.

Spectrochim. Acta A

Inorg. Chim. Acta

J. Organomet. Chem.

Z. Naturforsch. B

Inorg. Chem.

Z. Naturforsch. B

J. Chem. Soc.

Chem. Ber.

Z. Anorg. Allg. Chem.

Z. Anorg. Allg. Chem.

Chem.-Ztg.

Inorg. Chem.

Preparation, vibrational spectra and crystal structure of tris(trimethyltin) tetrathiophosphate (Me₃SnS)₃PS