Srinivasan, B. R., Girkar, S. V., Nather, C. and Bensch, Wolfgang (2009) Synthesis and structural characterization of bis(dimethylammonium) tetrasulfidometalates. Journal of Coordination Chemistry, 62 (22). pp. 3559-3572. DOI 10.1080/00958970903134282.

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Abstract

Reaction of (NH4)(2)[MS4] (M = Mo, W) with aqueous dimethylamine (CH3)(2)NH or KOH results in the formation of bis(dimethylammonium) tetrasulfidometalates [(CH3)(2)NH2](2)[MS4] (M = W 1; Mo 2) or dipotassium tetrasulfidotungstate K-2[WS4] (3). Compounds 1-3 were characterized by elemental analysis, IR and UV-Vis spectra and their crystal structures were determined. Compounds 1 and 2 are isostructural and crystallize in the centrosymmetric monoclinic space group P2(1)/n. The structures consist of two crystallographically independent dimethylammonium cations and a slightly distorted tetrahedral [MS4](2-) anion with all atoms situated in general positions. The cations and anions are involved in several weak N-H center dot center dot center dot S and C-H center dot center dot center dot S interactions. Compound 3 crystallizes in the centrosymmetric orthorhombic space group Pnma and is isostructural with the previously reported K-2[MoS4]. The structure of 3 consists of discrete slightly distorted tetrahedral [WS4](2-) anions of m symmetry, separated by two crystallographically independent K+ cations located on mirror planes. A comparative description of the alkali metal, ammonium, methyl and dimethylammonium tetrasulfidometalates is presented.

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