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化学学报
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化学学报 ›› 1999, Vol. 57 ›› Issue (4): 423-430. 上一篇    下一篇

研究论文

一些大取代二茂铁三碘化物的合成和结构分析

李金山;熊传辉;张经坤;刘成;白京生   

  1. 南开大学元素有机化学研究所.天津(300071);南开大学中心实验室.天津 (300071)
  • 发布日期:1999-04-15

Synthesis and structure analysis of some bulkily substituted ferrocenium triiodides

Li Jinshan;Xiong Chuanhui;Zhang Jingkun;Liu Cheng;Bai Jingsheng   

  1. Nankai Univ, Elementoorgan Chem Lab.Tianjin(300071);Nankai Univ, Ctr Lab.Tianjin(300071)
  • Published:1999-04-15

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合成了一系列大取代二茂铁三碘化物,通式为(RC~5H~4)~2FeI~3。通过元素分析,红外光谱,质谱,顺磁共振谱,穆斯堡尔谱和电导率对这些化合物进行了表征。测定了化合物[CH~2(CH~2)~3C(2-CH~2C~5H~4N)C~5H~4]~2FeI~4.H~2O的晶体结构,该晶体属三斜晶系,P-1空间群,晶胞参数:a=0.9593(1),b=1.3999(2),c=1.4537(2)nm。α=109.64(1),β=97.25(1),γ=104.69(1)ⅲ。V=1.7299nm^3,Mr=1030.13,Dx=1.98g/cm^3,Z=2。结果表明,取代二茂铁被碘部分氧化,导致中心金属铁表现为混合价态;由于茂环上大取代基的影响,使得I~3^-与I~3^-之间未能形成碘链,因此这些化合物的电导率很低。

关键词: 二茂铁, 碘化物, 晶体结构, 元素分析, 红外分光光度法, 质谱法, 顺磁共振, 穆斯堡尔谱法

A series of bulkily substituted ferrocenium triiodides with general formula (RC~5H~4)~2FeI~3 have been synthesized and characterized by elementary analysis, IR spectrum, mass spectrum, ESR spectrum, Mossbauer spectrum and conductivity. The crystal structure of [CH~2 (CH~2)~3C(2-CH~2C~5H~4N)C~5H~4]~2FeI~4.H~2O has been determined. The crystal belongs to triclinic, space group P-1, the cell parameters are a=0.9593(1), b=1.3999(2), c=1.4537(2)nm。α=109.64(1), β=97.25(1) , γ =104.69(1)ⅲ。V=1.7299nm^3, Mr=1030.13, Dx=1.98g/cm^3, Z=2. The results indicate that the substituted ferrocene is partially oxidized by iodine, therefore the central metal iron shows mixed valence state. Because of the effect of bulky substituents in cyclopentadienyl ring the polyiodide chains of the I~3^- ions are not formed, the conductivities of these compounds are very low.

Key words: FERROCENE, IODIDE, CRYSTAL STRUCTURE, ELEMENTAL ANALYSIS, INFRARED SPECTROPHOTOMETRY, MASS SPECTROGRAPHY, PARAMAGNETIC RESONANCE, MOSSBAUER SPECTROMETRY

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