化学学报 ›› 1995, Vol. 53 ›› Issue (3): 243-247. 上一篇    下一篇

研究论文

双(三甲硅基环戊二烯基羰基钼)配合物的合成和结构

邝代治;周秀中   

  1. 衡阳师范专科学校化学系;南开大学化学系
  • 发布日期:1995-03-15

Synthesis and stuctures of bis(trimethylsilylcyclopentadienyl carbonyl molybdenum)complexes

KUANG DAIZHI;ZHOU XIUZHONG   

  • Published:1995-03-15

通过三羰基(三甲硅环戊二烯基)钼负离子盐[η-M~e~3sic~5H~4Mo(CO)~3]^-Li~+氧化偶联合成了Mo-Mo键双核化合物(1),在甲苯中回流制得含Mo≡Mo 叁键化合物(2),乙炔对这Mo≡Mo键加成形成四面体形配合物(3),经元素分析.IR和~1HMR谱表征了标题化合物的结构.并用X射线衍射测定了配合物[η-M~e~3sic~5H~4Mo(CO)~3]~2(1)的晶体结构.1为单斜晶系,空间群为P2~1/c,晶体学数据:a=1.2826(2),b=0.8211(5),c=1.2902(1)nm,β=1.0480(2)°,V=1.3138nm^3,Z=2,D~ x= 1. 604g.cm^-^3,μ=10.530cm^-^1,F(000)=636.硅桥联双[三羰基(三甲硅基环戊二烯基)钼]负离子盐E[η-M~e~3sic~5H~4Mo(CO)~3]~2^2^-Li^+~2,[E=SiMe~2, O(SiMe~2)~2],也用类似方法合成化合物4,5,也经元素分析.IR.^1HNMR表征.

关键词: 红外分光光度法, 元素分析, 晶体结构, 质子磁共振谱法, 钼络合物, 耦合反应, 双核络合物, 双三甲硅基环戊二烯基羰基钼, 三甲硅基环戊二烯

The Mo-Mo bond dinuclear compounds were synthesized via oxidative coupling of tricarbonyltrimethylsilylcyclopentadienyl molybdenum anion salt and silylene-bridged bis(tricarbonyltrimethylsilylcyclopentadienylmolybdenum anion salts) E[h-Me3SiC5H3Mo(CO)3]22-Li2+, [E = SiMe2, O(SiMe2)2], resp. Compound containing molybdenum-molybdenum triple bond was also prepared by heating [h-Me2SiC5H4Mo(CO)3]2 (I) under reflux in toluene. Acetylene add to the MoYMo triple bond to give tetrahedron complex, structures of the title compounds were characterized by elemental analyses, IR and 1H NMR spectra. The crystal structures of complex I was determine

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, CRYSTAL STRUCTURE, PROTON MAGNETIC RESONANCE SPECTROMETRY, MOLYBDENUM COMPLEX, COUPLING REACTION, DINUCLEAR COMPLEX

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