Bis(piperazin-1-ium) tetrasulfidometalates: Solid state synthesis, thermal studies and structural characterization

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• 作者：Biksh ; arkoil R. Srinivasan ; Ashish R. Naik ; Martha Poisot ; Christian Nä ; ther ; Wolfgang Bensch
• 关键词：Tetrasulfidometalate ; Piperazin-1-ium ; N– ; H· ; · ; · ; N interactions ; Endothermic ; Piperazinediium
• 刊名：Polyhedron
• 出版年：2009
• 出版时间：12 May 2009
• 年：2009
• 卷：28
• 期：7
• 页码：1379-1385
• 全文大小：485 K

文摘

The organic tetrasulfidometalates (pipH)₂[MS₄] (pipH = piperazin-1-ium; M = W 1; M = Mo 2) were prepared by a mechanical grinding of solid (NH₄)₂[MS₄] (M = Mo or W) with the cyclic diamine piperazine (pip). Compounds 1 and 2 which contain the monoprotonated cation of piperazine were characterized by elemental analysis, infrared, Raman and UV–Vis spectra and their structures were determined. The title compounds decompose endothermically to carbon containing metal disulfide residues. Both compounds are isostructural and crystallize in the centrosymmetric triclinic space group . The structures of both compounds consist of two crystallographically independent piperazin-1-ium cations and a tetrasulfidometalate dianion, with all atoms situated in general positions. An intramolecular N–H···N interaction links the organic cations into pairs and the pairs thus formed extend into a one-dimensional chain of cations with the aid of an intermolecular N–H···N bond. The [MS₄]²⁻ anions are linked to the chains of piperazin-1-ium cations via N–H···S and C–H···S interactions. A comparative study of the spectral, structural and thermal properties of the title compounds with those of the previously reported (pipH₂)[MS₄] (pipH₂ = piperazinediium) compounds containing the (pipH₂)²⁺ dication is described.