高等学校化学学报

高等学校化学学报 ›› 1991, Vol. 12 ›› Issue (9): 1149.

• 论文 • 上一篇    下一篇

含低价钼的双核化合物(Et4N)2[(CO)4Mo(μ-S)2MOS2]和(Et4N)2[(CO)4Mo(μ-S)2WS2]的合成及晶体结构

余佩华1, 萧泰1, 庄伯涛2   

  1. 1. 西北师范大学化学系, 兰州, 730000;
    2. 中国科学院福建物质结构研究所
  • 收稿日期:1990-06-19 出版日期:1991-09-24 发布日期:1991-09-24
  • 通讯作者: 余佩华

Studies on Synthesis and Crystal Structure of the Mo(0) Binuclear Complexes (Et4N)2[(CO)4Mo(μ-S)2MS2](M=Mo,W)

Yu Pei-hua1, Xiao Tai1, Zhuang Bo-tao2   

  1. 1. Department of Chemistry, Northwest Normal University, Lanzhou, 730000;
    2. Fujian Institute of Research on the Structure of Matter, Academia Smica, Fuzhou
  • Received:1990-06-19 Online:1991-09-24 Published:1991-09-24

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摘要： 用新方法合成并测定了含Mo(0)的双核化合物(Et4N)2[(CO)4Mo(μ-S)2MOS2](Ⅰ)和(Et4N)2[(CO)4Mo(μ-S)2WS2](Ⅱ)的晶体结构.Ⅰ和Ⅱ空间群均为Pbcm,Ⅰ的a=1.8403(2)nm,b=1.1963(1)nm,c=1.3482(1)nm,Z=4,R=0.042;Ⅱ的a=1.8453(2)nm,b=1.2004(2)nm,c=1.3494(3)nm,Z=4,R=0.032,Ⅰ和Ⅱ的阴离子均为以Mo(0)为中心的八面体和以Mo(Ⅵ)(或W)为中心的四面体共边且以μ-S连接,Mo(μ-S)2M(M=Mo,W)共平面.其中Mo-Mo键距为0.2992(2)nm,Mo-W为0.30330(8)nm,并发现其FourierIR中Mo(0)-Sb键的v=424.3cm-1。

关键词: 含Mo(0)的双核簇合物, 合成, 晶体结构

Abstract: The Mo(0)binuclear complexes (Et4N)2[(CO)4Mo(μ-S)2MoS2](Ⅰ)and (Et<N)2[(CO)4Mo(μ-S)2WS2](Ⅱ) were synthesised with a new method, and their crystalline structures were determined by X-ray crystallography. Ⅰ and Ⅱ Crystallize in the orthogonal system and the space group is Pbcm with a=1. 8403(2), b=1.1963(1), c=1. 3482(1) nm, Z=4, R=0. 042 for Iand with α=1. 8453(2), 6=1.2004(2), c=1. 3482(3) nm, Z=4, R=0. 032 for I. The structures of the anions of Ⅰ and Ⅱ are all composed of both an octahedron around the Mo(0) atom and a tetrahedron with the Mo (Ⅵ) or W(Ⅵ) atom in the center by sharing an edge which is the line between the two bridged sulfur atoms. The bond distance of Mo-Mo is 0. 2992(2) nm and Mo-Wis 0. 3033(8) nm, and the bimetallic center Mo(μ-S)2M(M=Mo, W) is planar. It was found in the Fourier IRspectrum of complex Ⅱ that the absorption band of Mo(0)-Sb is v=424. 3 cm-1.

Key words: Mo(0) binuclear clusters, Synthesis, Crystal structure

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