Syntheses and structural characterizations of a series of Mo(W)–Cu–S compounds of bidentate dialkyldithiocarbamate ligands. Crystal structure of [NEt4]2[Mo2Cu5S6O2(Me2NCS2)3]
Abstract
The complex [NEt4]2[Mo2Cu5S6O2(Me2NCS2)3] has been prepared by the reaction of CuCl, Na[S2CNMe2],NEt4Br, and [NH4]2[MoS2O2] in dimethylformamide solution. It crystallizes in the orthogonal space group Pnma with a= 23.373(3), b= 17.202(3), c= 12.474(4)Å, and Z= 4. The Mo2Cu5S6O2 framework in the anion consists of two defective cubane-like units OMoS3Cu2 and OMoS3Cu3 linked through two weak Cu–S bonds and bridged by two Me2NCS2 ligands. The synthesis of the series of compounds [NEt4]2[M2Cu5S8(Me2NCS2)3], [PPh4]2[M2Cu5S6O2(Et2NCS2)3](M = Mo or W), and [NEt4]2[MoCu3S4(Et2NCS2)3] are reported. Their structures are discussed together with their 1H, 13C, and 95Mo n.m.r. spectra in solution.