高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (10): 1464.

• 论文 • 上一篇    下一篇

含柠檬酸配体的钼硫簇合物的合成与晶体结构的测定

李冬梅1, 李亚丰1, 邢永恒1, 王仁章1, 刘淑清1, 孙浩然1, 王铁钢1, 徐吉庆1,2, 邢燕3, 林永华3, 贾恒庆3   

  1. 1. 吉林大学化学系, 长春 130023;
    2. 南京大学配位化学国家重点实验室, 南京 210093;
    3. 中国科学院长春应用化学研究所, 长春 130022
  • 收稿日期:1999-06-18 出版日期:2000-10-24 发布日期:2000-10-24
  • 通讯作者: 徐吉庆(1937年出生),男,教授,博士生导师,从事原子簇化学研究.
  • 基金资助:

    国家自然科学基金(批准号:29733090);高等学校博士学科点专项科研基金及配位化学国家重点实验室资助

Synthesis and Structure of Molybdenum citrato Cluster μ2-S Bridge

LI Dong-Mei1, LI Ya-Feng1, XING Yong-Heng1, WANG Ren-Zhang1, LIU Shu-Qing1, SUN Hao-Ran1, WANG Tie-Gang1, XU Ji-Qing1,2, XING Yan3, LIN Yong-Hua3, JIA Heng-Qing3   

  1. 1. Departmentof Chemistry, Jilin University, Changchun 130023, China;
    2. State Key Laboratoryof Coordination Chemisty, Nanjing University, Nanjing 210093, China;
    3. Changchun Instituteof Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
  • Received:1999-06-18 Online:2000-10-24 Published:2000-10-24

摘要: 合成了含有Mo—S簇阴离子[Mo2O2(μ-S)2(C6H5O7)(C6H4O7)]5-柠檬酸簇合物,并通过元素分析、红外光谱、紫外-可见光谱和X射线光电子能谱对配合物进行了表征,用X射线衍射法测定了该化合物的晶体结构.结果表明,该簇合物属于单斜晶系,空间群P21/c,a=2.3766(5)nm,b=1.3274(3)nm,c=2.2471(5)nm,α=γ=90°,β=118.21°,V=6.247(2)nm3,Z=8,一致性因子R=0.0831,R2,w=0.1536.该簇合物阴离子中每一个Mo原子都采取扭曲的八面体结构,柠檬酸通过羟基、α-羧基、一个β-羧基与Mo配位.晶体结构表明在一个结晶学上不对称的结构单元内有两个结晶学上独立的分子.

关键词: 固氮酶, 柠檬酸, 合成, 晶体结构, 硫桥双核钼簇合物

Abstract: Anew molybdenum-citrato cluster containing [Mo2O2( μ-S)2(C6H5O7)(C6H4O7)]5- anion was synthesized and characterized by elemental analysis, IR, UV-Vis spectra, XPS and X-ray diffraction. The parameters of the crystal structure of the compound are monoclinic, space group P21/c, a =2.3766(5) nm, b =1.3274(3) nm, c =2.2471(5) nm, β =118.21°, V =6.247(2) nm3, Z=8, Dc=2.128 g/cm3, F(000)=3984, μ =1694 cm-1 , R=0.0831 and R2,w=0.1549. The anion is binuclear molybdenum citrato complex with μ2-S bridge. Each molybdenum atom pocesesses a distorted octahedral struture, which is coordinated with a terminal oxygen, two sulfur atoms, three oxygen atoms of hydroxyl, α-carboxylate, β-carboxylate from citrate.

Key words: Nitrogenase, Citric acid, Synthesis, Crystal structure, Binuclear molybdenum cluster with μ2-S bridge

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