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A cubane-type molybdenum cluster compound Mo4S4(DTP)4[-SOP(OEt)2]2 A (DTP = diethyl dithiophosphate) was obtained from the reaction of cation [Mo3O2S2(H2O)9]4+ B with metal tin as well as HDTP. The crystal structure has been determined by X-ray crystallography and the data for the title compound: Mo4S14P6O14C24H60, triclinic P , Mr = 1591.14, a = 12.5596(5), b = 14.3441(5), c = 18.0005(6) ? = 85.318(1), = 70.495(1), = 78.415(2)? V = 2994.2(2) ?, Z = 2, Dc = 1.765 g/cm3, (MoK? = 1.515 mm-1, F(000) = 1596, R = 0.0918 and wR = 0.1908 for 3546 reflections (I > 2(I)). X-ray analysis reveals that two weak CH贩稯 hydrogen bonds exist in the packing diagram with C贩稯 distance 3.22(5) ? The structure of A is similar to that of -Mo4S4(DTP)6 except that one sulfur of each bridging DTPs has been replaced by oxygen during the reaction, resulting in two bridging [SOP(OEt2)2] - ligands.
A cubane-type molybdenum cluster compound Mo4S4 (DTP) 4 [-SOP (OEt) 2] 2 A (DTP = diethyl dithiophosphate) was obtained from the reaction of cation [Mo3O2S2 (H2O) 9] 4+ B with metal tin as well as HDTP. The crystal structure has been determined by X-ray crystallography and the data for the title compound: Mo4S14P6O14C24H60, triclinic P, Mr = 1591.14, a = 12.5596 (5), b = 14.3441 (5), c = ) = 85.318 (1) = 70.495 (1) = 78.415 (2) • V = 2994.2 (2) • Z = 2 • Dc = 1.765 g / cm3 • MoK • = 1.515 mm-1 • F 000) = 1596, R = 0.0918 and wR = 0.1908 for 3546 reflections (I> 2 (I)). X-ray analysis reveals that two weak CHs. ) The structure of A is similar to that of -Mo4S4 (DTP) 6 except that one sulfur of each bridging DTPs has been replaced by oxygen during the reaction, resulting in two bridging [SOP (OEt2) 2] -labeleds.