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化学学报
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化学学报 ›› 1989, Vol. 47 ›› Issue (1): 25-30. 上一篇    下一篇

研究论文

含SR桥的双核钼(I)配合物Mo2(CO)8-n(SR)2Ln的新合成途径和Mo2(C(O)6(SPh)2(MeCN)2的结构研究

庄伯涛;黄梁仁;何玲洁;杨瑜;卢嘉锡   

  1. 中国科学院福建物质结构研究所
  • 发布日期:1989-01-15

New route to synthesize dinuclear Mo(I)complexes, Mo2(CO)8-n (μ -SR)2Ln and structure of No2(CO)6(μ-SPH)2(CH3CN)2

ZHUANG BOTAO;HUANG LIANGREN;HE LINGJIE;YANG YU;LU JIAXI   

  • Published:1989-01-15

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经由零价双核钼含SR桥的配合物的氧化反应合成了一系列含各种SR桥的双核钼(I)配合物Mo2-(CO)8-n(μ-SR)2Ln(R=Br^t, Ph, Bz(C6H5CH2), CH2CO2Et;L=MeCN, PPh3; n=0,2]. 并应用红外光谱、元素分析等进行表征, 讨论了新的合成途径. 含MeCN配位体配位到Mo(I)上的配合物, Mo2(CO)6(SPh)2(MeCN)2经X射线结构测定, 系属单斜晶系, 空间群P21/c,a=9.241(2), b=9.330(3), C=15.458(4)A:β=105.77(2)°V=1283(1)A^3; Z=2; R=0.033. Mo-Mo距离为2.978A, 表明其Mo-Mo距离为2.978A, 表明其Mo-Mo键的形成, Mo-S键长为2.469A. 比较同系物Mo2(CO)8(μ-SCH2CO2-Et)2, Mo2(CO)6(μ-SCH2CO2Et)2(MeCN)2和Mo2(CO)8(μ-SBu^t)2的结构, 并讨论其结构与化学.

关键词: 晶体结构测定, 分子结构, Ｘ射线衍射分析, 羰基络合物, 固氮酶, 钼络合物, 三苯基膦, 二苯基甲烷 P, 特丁基, 乙酸 P

Mo2(CO)8-n(m-SR)2Ln [R = Ph, Me3C, PhCH2, CH2CO2Et; L = MeCN, PPh3; n = 0, 2] were prepared by oxidation of (Et4N)2[Mo2(m-SR)2(CO)8] with I and characterized by elemental anal., IR spectroscopy and x-ray crystallog. A new route to prepare these Mo(I) complexes was discussed. The crystal and mol. structure of Mo2(CO)6(m-SPh)2(MeCN)2 was determine from 3-dimensional x-ray data. It crystallizes in the monoclinic, space group P21/c, a 9.241(2), b 9.330(3) c 15.458(4) ? b 105.77(2)? Z = 2, R = 0.033 for 1628 reflections with I>3s (I). The distance of Mo-Mo is 2.978 ?indicating formation of a Mo-Mo bond and the distance of the Mo-S bond is 2.469 ? In comparison with its analogs Mo2(CO)8(m-SCH2CO2Et)2, Mo2(CO)8(m-SCMe3)2 and Mo2(CO)6(m-SCH2CO2Et)2(MeCN)2, the structure relevant to its chem. was discussed.

Key words: CRYSTAL STRUCTURE DETERMINATION, MOLECULAR STRUCTURE, X-RAY DIFFRACTION ANALYSIS, CARBONYL COMPLEX, NITROGENASE, MOLYBDENUM COMPLEX, TRIPHENYLPHOSPHINE, DIPHENYLMETHANE P, TERT.-BUTYL GROUP, ACETIC ACID P

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