Key indicators: single-crystal X-ray study; T = 298 K; mean (C-C) = 0.009 Å; R factor = 0.050; wR factor = 0.100; data-to-parameter ratio = 17.3.The title compound, (C 8 H 12 N) 2 [MoS 4 ], was synthesized by the aqueous reaction of ammonium tetrathiomolybdate with benzyl(methyl)amine in a 1:2 molar ratio. The structure consists of a slightly distorted tetrahedral [MoS 4 ] 2À dianion and two crystallographically independent benzyl(methyl)ammonium cations, with all atoms located in general positions. The cations and anions are linked by weak N-HÁ Á ÁS and C-HÁ Á ÁS interactions, the strength and number of which can explain the observed Mo-S bond distances.
The synthesis and characterization of the bis(alkylammonium) tetrasulfidometalates, (EtNH 3 ) 2 [MS 4 ] (M¼ W 1, Mo 2), [BuNH 3 ] 2 [MS 4 ] (M¼ W 3; Mo 4) and (Et-enH 2 )[WS 4 ] 1-en (Et-en ¼ N-ethylethane-1,2-diamine), are reported. Compound 1 crystallizes in the centrosymmetric orthorhombic space group Pnma and its structure consists of discrete slightly distorted tetrahedral [WS 4 ] 2À of m symmetry, separated by two crystallographically independent (EtNH 3 ) þ ions located on mirror planes. The carbons of one ethylammonium are disordered. Compound 1-en crystallizes in the centrosymmetric orthorhombic space group Pbca with all atoms situated in general positions. Its structure consists of discrete (Et-enH 2 ) 2þ and a slightly distorted tetrahedral [WS 4 ] 2À with the cations and anions linked by several weak hydrogen bonds.
The title compound, (C8H12N)2[WS4], was synthesized by the aqueous reaction of ammonium tetrasulfidotungstate(VI) with benzyl(methyl)amine in a 1:2 molar ratio. The compound is isotypic with the corresponding Mo analogue, (C8H12N)2[MoS4], and its structure consists of a slightly distorted tetrahedral [WS4]2− dianion and two crystallographically independent benzyl(methyl)ammonium cations, with all atoms located in general positions. The cations and anion are linked by weak N—H...S and C—H...S interactions, the strength and number of which can explain the observed W—S bond distances.
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