Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo3S4 (dtp)3(o-CH3OC6H4COO)(Py) and Mo3S4 (dtp)3(p-HOC6H4COO)(DMF).EtOH

The title compounds Mo3S4(dtp)3(o-CH3OC6H4COO)(Py) 1 and Mo3S4 (dtp)3(p-HOC6H4COO)(DMF)·EtOH 2 (dtp = diethyldithiophosphate) were synthesized by the reactions of Mo3S4(dtp)4(CH3CN) and Mo3S4(dtp)3(CH2ClCOO)(Py) with o-methoxylbenzoic acid and p-hydroxybenzoic acid, respectively. Their crystal structures were determined by X-ray diffraction analysis. The crystal data for compound 1: Mo3S10P3C25H42O9N, monoclinic P21/n, Mr = 1201.93, Z = 4, a = 14.164(1), b = 23.065(2), c = 14.732(1) A, β = 109.677(1)°, V = 4532(1) A3, Dc = 1.762 g cm-3, μ = 1.428 mm-1, F(000) = 2408, R = 0.0739, wR = 0.1528 for 3552 observed reflections (I > 2σ); and for compound 2: Mo3S10P3C24H48O11N, triclinic P ī, Mr = 1227.96, Z = 2, a = 10.2098(3), b = 14.3333(4), c = 18.1711(5) A, α = 94.694(1), β = 102.166(1), γ = 110.665(1)°, V = 2396.5(1)A3, Dc = 1.638 g cm-3, μ = 1.350mm-1, F(000) = 1184, R = 0.0445, wR = 0.1281 for 6597 observed reflections (I > 2σ). Intermolecular S…S interactions are observed between the molecules of compound 1 while intramolecular O…H-C and intermolecular S…H-C hydrogen bondings are found in the crystal packing diagram of compound 2.