Syntheses, Crystal Structures of Mo–S Clusters [Mo3S4(dtp)3(L)]2[μ-OOC(CH2)nCOO-μ] (L = dmf, dmso; n = 3, 4) and Their Supramolecular Architectures

The substitution reaction of ‖Mo 3 S 4 (dtp) 3 (ClCH 2 COO)(py)] (dtp = diethyl dithiophosphate) or [Mo 3 S 4 (dtp) 4 -(H 2 O)‖ with adipic acid or glutaric acid in N,N'-dimethylformamide (dmf) or dimethyl sulfoxide (dmso) dimerized two discrete Mo 3 S 4 clusters into novel Mo(IV) cluster compounds [Mo 3 S 4 (dtp) 3 (L) 2 [μ-OOC(CH 2 ) n COO-μ] (L = dmf, n = 4 for 1. n = 3 for 2; L = dmso, n = 3 for 3). Their structures have been determined by X-ray crystallography and spectroscopically characterized. Each molecule of these clusters consists of two incomplete cubane-type [Mo 3 S 4 (dtp) 3 (L)] units, and each unit is respectively coordinated to one dicarboxylale group of the same dicarboxylic acid. Intermolecular SS and C-HS contacts, observed in the crystal packing diagram, establish three infinite two-dimensional supramolecular architectures.