Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py)

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The title compounds Mo3S4(dtp)3(o-CH3OC6H4COO)(Py) 1 and Mo3S(dtp)3(p-HOC6H4COO)(DMF)稥tOH 2 (dtp = diethyldithiophosphate) were synthesized by thereactions 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) ? = 109.677(1) ? V = 4532(1) ?, D= 1.762 gcm-3, = 1.428 mm-1, F (000) = 2408, R = 0.0739, wR = 0.1528 for 3552 observed reflections (I > 2); and for compound 2: Mo3S10P3C24H48O11N, triclinic P ? Mr = 1227.96, Z = 2, = 10.2098(3), b = 14.3333(4), c = 18.1711(5) ? = 94.694(1), = 102.166(1), = 110.665(1) , V = 2396.5(1)3, Dc = 1.638 gcm-3, = 1.350mm-1, F (000) = 1184, R = 0.0445, wR = 0.1281 for 6597 observed reflections (I > 2). Intermolecular S…S interactions are observed between the molecules of compound 1 while intramolecular O…HC and intermolecular S…HC hydrogen bondings are found in the crystal packing diagram of compound 2. The title compounds Mo3S4 (dtp) 3 (o-CH3OC6H4COO) (Py) 1 and Mo3S (dtp) 3 (p-HOC6H4COO) (DMF) 稥 tOH 2 (dtp = diethyldithiophosphate) were synthesized by thereaction 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)? = 109.677 (1)? V = 4532 -3 = 1.428 mm -1, F (000) = 2408, R = 0.0739, wR = 0.1528 for 3552 observed reflections (I> 2); and for compound 2: Mo3S10P3C24H48O11N, triclinic P = Mr = 1227.96, Z = 2 (1), = 10.2098 (3), b = 14.3333 (4), c = 18.1711 (5) = 94.694 (1), = 102.166 (1), = 110.665 (1), V = 2396.5 Intermolecular S ... S interactions are observed between the molecules of compo (I> 2) gcm-3, = 1.350 mm -1, F (000) = 1184, R = 0.0445, wR = 0.1281 for 6597 observed reflections und 1 while intramolecular O ... HC and intermolecular S ... HC hydrogen bondings are found in the crystal packing diagram of compound 2.
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