The reaction of Mo(CO)6 with m-CH_3-C6H4SNa and Et4NCl(H_2O in CH_3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-m)2] (1). The crystal structure was determined by X-ray crystallography. Th...The reaction of Mo(CO)6 with m-CH_3-C6H4SNa and Et4NCl(H_2O in CH_3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-m)2] (1). The crystal structure was determined by X-ray crystallography. The crystallographic data: C38H54Mo2N2O8S2, Mr = 922.87, triclinic, P_ 1, a =10.336(2), b=10.753(2), c=11.121(2) ?, ( =88.88(2), ( =68.64(1), ( =69.71(1)(, V=1071.5(1) ?3, Z=1, Dc=1.43 g/cm3, F(000) = 476, ( = 7.1cm－1, Final R = 0.036 and Rw = 0.045 for 3423 reflections with I >3.0( (I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distorted octahedron, both of which form an edge-sharing bioctahedron. The Mo...Mo distance is 4.0665(1)(, which obviously indicates the absence of Mo-Mo bond.展开更多
The reaction of [Et4N]2[Mo2(SC6H11)2(CO)8] and I2 in MeCN affords a new dinu- clear molybdenum(I) complex [Mo2(SC6H11)2(CO)6(CH3CN)2] 1 (Mr = 672.46). The crystal and molecular structures have been determined by X-r...The reaction of [Et4N]2[Mo2(SC6H11)2(CO)8] and I2 in MeCN affords a new dinu- clear molybdenum(I) complex [Mo2(SC6H11)2(CO)6(CH3CN)2] 1 (Mr = 672.46). The crystal and molecular structures have been determined by X-ray single-crystal diffraction. 1 crystallizes in monoclinic, space group P21/c with a = 9.302(1), b = 15.514(2), c = 9.307(1) ?, β = 92.979(2)o, V = 1341.4(3) ?3, Z = 2, Dc = 1.665 g/cm3, μ = 11.28 cm-1, F(000) = 676, R = 0.0461 and wR = 0.1274 for 1702 observed reflections with I > 2σ(I). 1 possesses a rhombic bimetallic core MoS2Mo with the Mo–Mo bond length of 2.9712(4) ? and Mo–S of 2.4821(5) ?.展开更多
A new trithiocarbonato Mo complex(Et_4N)_2[(S_2)Mo2O_2(μ-S)_2(CS_3)]was obtained from a system containing MoO_4^(2-),S_x^(2-),and CS_2 and characterized by IR and X-ray structural analysis. The complex crystallizes i...A new trithiocarbonato Mo complex(Et_4N)_2[(S_2)Mo2O_2(μ-S)_2(CS_3)]was obtained from a system containing MoO_4^(2-),S_x^(2-),and CS_2 and characterized by IR and X-ray structural analysis. The complex crystallizes in the (?)onoclinic space group P2_1/c with a=9.539(3)(?), b=20.745(2)(?),c=15.452(2)(?),β=94.58(2)°,and Z=4.The structure was solved by direct and difference Fourier synthesis methods.Least squares refinement using 2910 reflections with I>3σ(I)converged to R=0.054.The CS_3^(2-) iigand in the complex chelates to Mo atom and values of the C-S bond distances in the CS_3^(2-) ligend indicate a substantial contribution of three resonance forms.展开更多
文摘The reaction of Mo(CO)6 with m-CH_3-C6H4SNa and Et4NCl(H_2O in CH_3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-m)2] (1). The crystal structure was determined by X-ray crystallography. The crystallographic data: C38H54Mo2N2O8S2, Mr = 922.87, triclinic, P_ 1, a =10.336(2), b=10.753(2), c=11.121(2) ?, ( =88.88(2), ( =68.64(1), ( =69.71(1)(, V=1071.5(1) ?3, Z=1, Dc=1.43 g/cm3, F(000) = 476, ( = 7.1cm－1, Final R = 0.036 and Rw = 0.045 for 3423 reflections with I >3.0( (I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distorted octahedron, both of which form an edge-sharing bioctahedron. The Mo...Mo distance is 4.0665(1)(, which obviously indicates the absence of Mo-Mo bond.
文摘The reaction of [Et4N]2[Mo2(SC6H11)2(CO)8] and I2 in MeCN affords a new dinu- clear molybdenum(I) complex [Mo2(SC6H11)2(CO)6(CH3CN)2] 1 (Mr = 672.46). The crystal and molecular structures have been determined by X-ray single-crystal diffraction. 1 crystallizes in monoclinic, space group P21/c with a = 9.302(1), b = 15.514(2), c = 9.307(1) ?, β = 92.979(2)o, V = 1341.4(3) ?3, Z = 2, Dc = 1.665 g/cm3, μ = 11.28 cm-1, F(000) = 676, R = 0.0461 and wR = 0.1274 for 1702 observed reflections with I > 2σ(I). 1 possesses a rhombic bimetallic core MoS2Mo with the Mo–Mo bond length of 2.9712(4) ? and Mo–S of 2.4821(5) ?.
文摘A new trithiocarbonato Mo complex(Et_4N)_2[(S_2)Mo2O_2(μ-S)_2(CS_3)]was obtained from a system containing MoO_4^(2-),S_x^(2-),and CS_2 and characterized by IR and X-ray structural analysis. The complex crystallizes in the (?)onoclinic space group P2_1/c with a=9.539(3)(?), b=20.745(2)(?),c=15.452(2)(?),β=94.58(2)°,and Z=4.The structure was solved by direct and difference Fourier synthesis methods.Least squares refinement using 2910 reflections with I>3σ(I)converged to R=0.054.The CS_3^(2-) iigand in the complex chelates to Mo atom and values of the C-S bond distances in the CS_3^(2-) ligend indicate a substantial contribution of three resonance forms.
