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化学学报
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化学学报 ›› 1992, Vol. 50 ›› Issue (12): 1200-1205. 上一篇    下一篇

研究论文

1,1'-(四甲基二硅氧撑)双[环戊二烯基羰基钼配合物]的合成及结构

金仁志;徐善生;周秀中;王宏根;王如骥   

  1. 南开大学化学系;南开大学中心实验室
  • 发布日期:1992-12-15

Synthesis and structure of 1,1-(tetramethyl disiloxandiyl)bis [cyclopentadienyl carbonyl molybdenym complex]

JIN RENZHI;XU SHANSHENG;ZHOU XIUZHONG;WANG HONGGEN;WANG RUJI   

  • Published:1992-12-15

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312

被引次数

1

以1,3-二环戊烯基四甲基二硅氧烷相继与n-BuLi及Mo(CO)~6反应生成1,1'-(四甲基二硅氧撑)双[环戊二烯基羰基钼负离子盐](I),I分别与多种卤化物反应生成在钼原子上引入其它基团的衍生物,(Me~2SiOSiMe~2)[C~5H~4Mo(CO)~3R]~2.以元素分析、IR及^1HNMR谱表征了这些化合物的结构,并对其中之一的单晶(R=1)进行了X射线衍射分析.晶体属单斜晶系,P2~1/n空间群,晶体学数据,a=0.8707(2),b=1.0746(4),c=2.9719(8)nm,β=91.18(2)°,Ⅴ=2.7799nm^3,z=4,D~c=2.09g.cm^-3.最终偏差因子R为0.067.

关键词: 晶体结构测定, 红外分光光度法, 元素分析, Ｘ射线衍射分析, 硅氧烷, 环戊二烯 P, 质子磁共振谱法, 钼络合物, 丁基锂, 羟基化合物

1,3-Dicyclopentadienyltetramethyldisiloxane reacted sequentially with BuLi and Mo(CO)6 to generate 1,1'-(tetramethyldisiloxanediyl)bis[cyclopentadienyltricarbonylmolybdenu m anion salt], (Me2SiOSeMe2) [C5H4Mo(CO)3-Li+]2, (I). I reacted with RX (R = Me, Et, PhCH2, CH2CO2Et; X = halogen) to yield the corresponding molybdenum derivatives II. Their structures were characterized by elemental anal., IR and 1H NMR spectra. The crystal and mol. structure of II (R = iodo) was determine by x-ray diffraction method.

Key words: CRYSTAL STRUCTURE DETERMINATION, INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, X-RAY DIFFRACTION ANALYSIS, SILOXANE, CYCLOPENTADIENE P, PROTON MAGNETIC RESONANCE SPECTROMETRY, MOLYBDENUM COMPLEX, BUTYLLITHIUM, HYDROXYL COMPOUNDS

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