高等学校化学学报

高等学校化学学报 ›› 1996, Vol. 17 ›› Issue (2): 231.

• 论文 • 上一篇    下一篇

柄型金属有机化合物(Ⅱ)──硅氧硅桥联二(1-茚基及四氢茚基)二氯化锆的合成和结构

王佰全1, 徐善生1, 周秀中1, 胡宁海2   

  1. 1. 南开大学化学系, 天津 300071;
    2. 中国科学院长春应用化学研究所
  • 收稿日期:1995-02-16 出版日期:1996-02-24 发布日期:1996-02-24
  • 通讯作者: 周秀中
  • 作者简介:王佰全,男,27岁,博士研究生.
  • 基金资助:

    国家自然科学基金;国家教育委员会博士点基金

Ansa-Metallocene Derivatves(Ⅱ)──Syntheses and Structures of Tetramethyldisiloxandiyl Bis(1-indenyl and tetrahydroindenyl)Zirconium Dichlorides

WANG Bai-Quan1, XU Shan-Sheng1, ZHOU Xiu-Zhong1, HU Ning-Hai2   

  1. 1. Department of Chemistry, Nankai University, Tianjin 300071;
    2. Changchun Institute of Applied Chemistry, Academia Sinica
  • Received:1995-02-16 Online:1996-02-24 Published:1996-02-24

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被引次数

19

摘要： 1,3-二(1-茚基)四甲基二硅氧烷相继与丁基锂及ZrCl4·2THF作用,生成硅氧硅桥联二(1-茚基)二氯化锆(Me2SiOSiMe2)[Ind]2ZrCl2(1).对其进行催化氢化得到相应的四氢茚基化合物(Me2SiOSiMe2)[IndH4]2ZrCl2(2).1和2均含有顺式和反式二种异构体(1c和1t以及2c和2t),通过重结晶得到纯的单一异构体1t、2c和2t,1c和2t的晶体结构经X射线衍射测定,二者均属单斜晶系,P21/n(1t)和P21/c(2c)空间群,其中2c分子的一个配体六元环在晶胞中具有两种几率完全相等的不同构象。

关键词: 柄型金属有机化合物, X射线衍射分析, 二茂锆化合物, 构象

Abstract: The ansa-zirconocene derivative tetramethyldisiloxandiyl bis(1-indenyl) zirconium dichloride(1) has been prepared by the reaction of the dilithium salt of 1,3-bis(1-indenyl) tetramethyldisiloxane with ZrCl4·2THF.After catalytic hydrogenation,the corresponding tetrahydroindenyl complex(2) has been formed.Both 1 and 2 have been shown by1H NMRspectra to be the mixture of the cis(meso) and trans(rac) isomers.The pure trans isomers 1t,2t and cis isomer 2c were obtained by recrystallization. The crystal structures of 1t and 2c were determined by X-ray diffraction. Both crystals of 1t and 2c are monoclinics,belonging to space groups P21/n(1t)and P21/c(2c).In the unit cell of 2c,one of the six-membered rings of the tetrahydroindenyl ligands has two different conformations which have the same probabilities.

Key words: ansa-Metallocene, X-ray diffraction, Zirconocene, Conformation

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