高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (10): 1833.

• 研究论文 • 上一篇    下一篇

钛锆钒异核双金属配合物[Cp2V(μ-η24-PhC4Ph)MCp2′](M=Ti,Zr;Cp′=C5H5,C5H4SiMe3)的合成与表征

赵建社1, 顾爱萍1, 何水样1, Robert Choukroun2, Lydie Valade2, Patrick Cassoux2   

  1. 1. 西北大学化学系, 西安 710069;
    2. 法国国家科研中心配位化学实验室, 法国图卢兹 31062
  • 收稿日期:2002-01-17 出版日期:2002-10-24 发布日期:2002-10-24
  • 通讯作者: 赵建社(1955年出生),男,博士,教授,从事金属有机和材料化学研究.E-mail:Jszhao@nwu.edu.cn E-mail:Jszhao@nwu.edu.cn
  • 基金资助:

    国家自然科学基金(批准号:20071027);陕西省科委自然科学基金(批准号:2000H04);陕西省教育厅专项基金(批准号:00JK130);1999年教育部留学回国人员基金资助

Synthesis and Crystal Structure of Heterodimetallic Complexes[Cp2V(μ-η2∶η4-PhC4Ph)MCp2′](M=Ti,Zr;Cp′=C5H5,C5H4SiMe3)

ZHAO Jian-She1, GU Ai-Ping1, HE Shui-Yang1, Choukroun Robert2, Valade Lydie2, Cassoux Patrick2   

  1. 1. Department of Chemis tr y, Northwest University, X i′an 710069, China;
    2. Laboratory of Coordination Chemistry, CNRS, F-31077 Toulouse, France
  • Received:2002-01-17 Online:2002-10-24 Published:2002-10-24

摘要: 室温下,[Cp2Ti(C≡CPh)2],[Cp2Zr(C≡CPh)2]和[(C5H4SiMe3)2Zr(C≡CPh)2]分别与二茂钒作用,合成了[Cp2V(μ-η2∶η4-PhC4Ph)MCp2′](1,M=Ti,Cp′=C5H5;2,M=Zr,Cp′=C5H5;3,M=Zr,Cp′=C5H4SiMe3).用元素分析、质谱、核磁共振谱、磁矩、红外和拉曼光谱对配合物进行了表征.3个配合物具有相似的磁化率,配合物3的晶体结构分析表明PhC4Ph通过内部2个碳原子键合到Cp2V上,内部2个碳原子和外部2个碳原子均与Cp2′Zr键合,丁二烯骨架内部的2个碳原子都具有四配位的平面结构.

关键词: 异核双金属配合物, 结构解释, 钛, 锆,

Abstract: The reaction of [Cp2Ti(C≡CPh)2], [Cp2Zr(C≡CPh)2], [(C5H4SiMe 3)2Zr(C≡CPh)2] and vanadocene in toluene was performed at room temperature and gave heterodimetallic complexes[Cp 2V(μ-η2∶η4-PhC4Ph)·MCp2′] (1, M=Ti, Cp′=C5H5; 2, M=Zr, Cp′=C5H5; 3, M=Zr, Cp′=C5H4SiMe3), respectively. These compounds, which have been characterized by elemental analysis, mass spectrometry, 1H NMR, IR and Raman spectroscopy, exhibit similar magnetic susceptibilities. According to an X-ray diffraction analysis of compound 3, the Cp2V and Cp2′Zr metallocene moieties are bonded to a butadiene(or butadiyne) framework via the two internal carbon atoms for Cp2V, and via both the two internal carbon atoms and the two external carbon atoms for Cp2′Zr. The distances and angles observed around the internal carbon atoms of the butadiene framework indicate that both internal carbon atoms of butadiene skeleton are planar and tetracoordinated.

Key words: Heterodimetallic complexes, Structure elucidation, Titanium, Zirconium, Vanadium

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