高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (8): 1515.

• 研究论文 • 上一篇    下一篇

新型桥联双四面体簇合物的合成与表征

张玉华1, 李庆山1, 夏春谷1, 殷元骐1, 周忠远2   

  1. 1. 中国科学院兰州化学物理研究所羰基合成与选择氧化国家重点实验室, 兰州 730000;
    2. 香港理工大学应用生物及化学技术学系, 香港
  • 收稿日期:2001-05-18 出版日期:2002-08-24 发布日期:2002-08-24
  • 通讯作者: hcom@ns.lzb.ac.cn
  • 作者简介:殷元骐(1932年出生),男,研究员,博士生导师,从事金属原子簇化学研究.E-mail:hcom@ns.lzb.ac.cn
  • 基金资助:

    国家自然科学基金(批准号:29871061)资助

Synthesis and Characterization of Novel Linked Clusters

ZHANG Yu-Hua1, LI Qing-Shan1, XIA Chun-Gu1, YIN Yuan-Qi1, ZHOU Zhong-Yuan2   

  1. 1. State Key Laboratory for Oxo Synthesis and Selective Oxidation, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China;
    2. Department of Applied Biology&Chemical Technology, The Hong Kong Polytechnic University, Hong Kong, China
  • Received:2001-05-18 Online:2002-08-24 Published:2002-08-24

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被引次数

2

摘要： 利用(μ3-CCO2Et)Co3(CO)9与单阴离子试剂[Mo(CO)3(η5-C5H4R)]-[R=H,C(O)Me]的反应合成了2个新的含CCo2Mo骨架的簇合物(μ3-CCO2Et)Co2Mo(CO)8(η5-C5H4R)[R=H(1);R=C(O)Me(2)],进而用其与双阴离子试剂{-M(CO)3[η5-C5H4C(O)]}2-1,4-C6H4[M=Mo,W]反应合成了4个双四面体簇合物{(μ3-CCO2Et)CoMoM(CO)7(η5-C5H4R)[η5-C5H4C(O)]}2-1,4-C6H4[M=Mo,R=H(3);M=Mo,R=C(O)Me(4);M=W,R=H(5);M=W,R=C(O)Me(6)].这6个化合物的C和H元素分析,IR,1HNMR等表征都与其结构一致.晶体X射线衍射分析表明,化合物2属单斜晶系,C2/c空间群,晶胞参数a=1.1264(3)nm,b=1.1879(3)nm,c=3.3565(10)nm,β=93.320(5)°,V=4.484(2)nm3,Z=8,Dc=1.867g·cm-3,F(000)=2480,R=0.0369,wR=0.1150.

关键词: 合成, 晶体结构, 簇合物, 钼, 金属交换反应

Abstract: The reactions of (μ3 CCO2Et)Co3(CO)9 with [Mo(CO)3 (η5 C5H4R)] - [R=Hor C(O)Me] gave rise to the formation of (μ3 CCO2Et)Co2Mo(CO)8 (η5 C5H4R) (1), C(O)Me(2)]. The further reaction of cluster 1 or 2. The further reaction of cluster 1 or 2 with {(M(CO)3[ η5 C5H4C(O)]}21, 4 C6H4 yielded four linked clusters { (μ3 CCO2Et)CoMoM(CO)7 (η5 C5H4R)[ η5 C5H4C(O)]}21, 4 C6H4 [M=Mo, R=H[STHZ](3); M=Mo, R=C(O)Me(4); M=W, R=H(5); M=W, R=C(O)Me(6)].. All these clusters were characterized by C/Hanalyses, IRand 1H NMR. The crystal structure of cluster 2 was determined by single crystal X-ray diffraction method. The crystal belongs to monoclinic system with space group, C2/c and lattice parameters, a=1.1264(3) nm, b=1.1879(3) nm, c=3.3565(10) nm, β =93.320(5)°, V=4.484(2) nm3, Z=8, Dc=1.867 g·cm-3, F(000)=2480, R=0.0369, wR= 0.1150.

Key words: Synthesis, Crystal structure, Cluster, Molybdenium, Metal exchange reaction

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