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化学学报
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化学学报 ›› 1997, Vol. 55 ›› Issue (8): 829-832. 上一篇    

研究论文

1,'-(四甲基二硅)桥联双(四甲基环戊二烯基)二氯化钛的合成和结构

徐善生;邓小斌;王佰全;周秀中   

  1. 南开大学化学系
  • 发布日期:1997-08-15

Synthesis and structure of 1,1'-(tetramethyldisilandiyl) bis (tetramethylcyclopentadienyl) titanium dichloride

XU SHANSHENG;DENG XIAOBIN;WANG BAIQUAN;ZHOU XIUZHONG   

  • Published:1997-08-15

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以1,2-二氯四甲基二硅烷与四甲基环戊二烯基锂反应, 生成1,2-二(四甲基环戊二烯基)四甲基二硅烷 (1)。1经正丁基锂处理后与TiCl4.2THG作用合成了标题化合物[Me2Si]2[η^5-C5Me4]2TiCl2 (2), 通过元素分析、UV、MS和^1H NMR谱表征了分子结构, 并对其单晶进行了X射线衍射分析。该晶体属于单斜晶系, 空间群C2/c, 晶胞参数: a=1.5060(3), b=0.9591(2),c=1.7490(3)nm; β=107.91(2)°, V=2.404(2)nm^3, Z=4, Dc=1.314g/cm^3,μ=6.80cm^-^1, F(000)=1008, R=0.047。

关键词: 紫外分光光度法, 元素分析, Ｘ射线衍射分析, 质谱法, 四氯化碳, 环戊二烯 P, 质子磁共振谱法, 金属茂络合物, 硅烷 P, 氯化钛

From the reaction of 1,2-dichlorotetramethyldisilane with tetramethylcyclopentadienyl lithium, 1,2-bis(tetramethylcyclopentadienyl) tetramethyldisilane (1) was formed. 1 was treated with n-butyl lithium and followed by reacting with tiCl4.2THF, the title compound 2 was obtained. Its structure was characterized by elemental analysis, UV, MS, ^1H NMR spectra and determined by X-ray diffraction analysis. The crystal belongs to monoclinic, space group C2/c. The parameters of the crystal are: a=1.5060(3), b=0.9591(2), c=1.7490(3)nm; β=107.91(2)°, V=2.404(2)nm^3, Z=4, Dc=1.314g/cm^3, μ=6.80cm^-^1, F(000)=1008, R=0.047.

Key words: ULTRAVIOLET SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, X-RAY DIFFRACTION ANALYSIS, MASS SPECTROGRAPHY, CARBON TETRACHLORIDE, CYCLOPENTADIENE P, PROTON MAGNETIC RESONANCE SPECTROMETRY, METALLOCENES, SILANE P, TITANIUM CHLORIDE

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