有机化学 ›› 1993, Vol. 13 ›› Issue (6): 627-632. 上一篇    下一篇

研究论文

溴钼环卡宾配合物的合成及结构

周秀中;邝代治;徐善生;张殿坤   

  1. 南开大学化学系.天津(300071);南开大学元素有机化学研究所.天津(300071)
  • 发布日期:1993-12-25

Syntheses and structures of bromomolybdenum cyclicarbene complexes

Zhou Xiuzhong;Kuang Daizhi;Xu Shansheng;Zhang Diankun   

  1. Nankai Univ, Dept Chem.Tianjin(300071);Nankai Univ, Elementoorgan Chem Lab.Tianjin(300071)
  • Published:1993-12-25

本文以三羰基戊二烯基钼负离子锂盐代替钠盐,成功地制得了溴钼环卡宾配合物。用X射线衍射测定了其晶体,晶体属正交晶系,空间群P2~12~12~1,晶体学数据:a=0.8600(2),b=1.4775(3),c=1.9900(7)nm;V=2.529nm^3,Z=8,D~x=1.93g.cm^-^3;μ=41.3cm^-^1,F(000)=1424。偏差因子R=0.055,R~w=0.060。

关键词: 羰基, 负离子, 合成, X射线衍射分析, 晶体结构, 环卡宾配合物, 环戊二烯基, 钼,

The title complexes were synthesized by reaction of (η -C~5H~4R)(CO) ~3) Mo^-Li^+ (R: H, SiMe~3, Si~2Me~5) with X(CH~2)~3X(X: Br, I) in THF. Their structures were characterized by elemental analyses, IR, ^1H NMR and ^1^3C NMR spectra. The crystal structure of η -C~5H~5(CO) ~2MoBrCO(CH~2)~CH~2 was determined by X-ray diffraction. The crystals are orthorhombic, space group P2~12~12~1, with a=0.8600(2), b=1.4775 (3), c=1.9900(7)nm; V=2.529nm^3, Z=8, D~x=1.93g.cm^-^3; μ=41.3cm^-^1, F(000)=1424. The final deviation factor R=0.055, R~w=0.060.

Key words: MOLYBDENUM, SYNTHESIS, CYCLOPENTADIENYL GROUP, BROMINE, ANIONS, CRYSTAL STRUCTURE, CARBONYL GROUP, X- RAY DIFFRACTION ANALYSIS

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