高等学校化学学报

高等学校化学学报 ›› 1999, Vol. 20 ›› Issue (12): 1827.

• 论文 •    下一篇

Co3(CO)7(μ3-S)(μ,η2-SCNR2)的合成和晶体结构

李松波1, 刘树堂1, 胡襄1, 吴秉芳1, 常菲1, 邢彦2, 贾恒庆2, 白石英2, 林永华2   

  1. 1. 内蒙古大学化学系, 呼和浩特 010021;
    2. 中国科学院长春应用化学研究所, 长春 130022
  • 收稿日期:1999-04-27 出版日期:1999-12-24 发布日期:1999-12-24
  • 通讯作者: 刘树堂
  • 作者简介:李松波,男,27岁,硕士,助教,现在内蒙古钢铁学院工作.
  • 基金资助:

    国家自然科学基金(批准号:29661001)资助课题

Syntheses and Crystalline Structures of Clusters Co3(CO)7(μ3-S)(μ,η2-SCNR2)

LI Song-Bo1, LIU Shu-Tang1, HU Xiang1, WU Bing-Fang1, CHANG Fei1, XING Yan2, JIA Heng-Qing2, BAI Shi-Ying2, LIN Yong-Hua2   

  1. 1. Department of Chemistry, Inner Mongolia University, Huhehaote 010021, China;
    2. Changchun Institute of Applied Chemistry, Academia Sin ica, Changchun 130022, China
  • Received:1999-04-27 Online:1999-12-24 Published:1999-12-24

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摘要： Co2(CO)8与4个二硫代双(烷基硫代甲酰胺)类前配体[R2NC(S)S]2反应,得4个含烷基硫代甲酰胺基的三核钴羰基硫簇合物.通过元素分析、IR、1HNMR和MS等方法表征了它们的结构,用X射线衍射法测定了其中一个簇合物Co3(CO)7(μ3-S)[μ,η2-SCN(i-Pr)2](Ⅲ)的晶体结构.晶体属单斜晶系,P21/n空间群,晶胞参数a=1.1452(2)nm,b=1.5028(3)nm,c=1.2144(2)nm,α=90°,β=92.15(3)°,γ=90°,V=2.0885(7)nm3,Z=4,F(000)=1096,Dc=1.747mg·m-3,GOF(F2)=0.835,μ=2.588nm-1.最终因子R[I>2σ(I)]=0.0407,Rw=0.0624.

关键词: 钴羰基硫簇合物, 二硫代双(烷基硫代甲酰胺)配体, 合成, 晶体结构

Abstract: Through the reaction of Co2(CO)8with four thiuram [R2NC(S)S]2, four new sulfur capped trinuclear cobalt carbonyl clusters Co3(CO)7(μ3-S)(μ,η2-S *C*NR2)(Ⅰ: R=Me; Ⅱ: R=Et; Ⅲ: R= i-Pr; Ⅳ: NR=, were prepared and characterized by elementary analysis, IR, 1HNMR and MS spectroscopy. The crystal structure of the cluster Co3(CO)7(μ3-S)[μ,η2-S*C*N(i-Pr)2] (Ⅲ) was determined by X-ray single crystal diffraction method. The crystal of Ⅲ is monoclinic, belonging to space group P21/n, and the cell parameters are as follows: a =1.1452(2) nm, b =1.5028(3)nm, c =1.2144(2) nm; α=90°, β=92.15(3)°, γ=90°; V=2.0885(7) nm3, Z =4, F(000)=1096, Dc=1.747 mg·m-3, μ=2.588 mm-1, R =0.0407, Rw=0.0624. The structural analysis shows that cluster Ⅲ has a pyrimidal Co3S framework and contains a heterocylic bridging bidentate ligand[μ,η2-S*C*N(i-Pr)2] linked to the Co2 and Co3 atoms of the cluster by a cobalt-carbon and a cobalt-sulfur bond respectively.

Key words: Sulfo-trinuclear cobalt cluster, Thiuram ligand, Synthesis, Crystal structure

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