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化学学报
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化学学报 ›› 1990, Vol. 48 ›› Issue (9): 867-872. 上一篇    下一篇

研究论文

砷硫桥羰基铁配合物(μ-Ph2As)(μ-RS)Fe2(CO)6的合成及结构

宋礼成;王如骥;李宇;王宏根;王积涛   

  1. 南开大学测试计算中心
  • 发布日期:1990-09-15

Synthesis and structures of iron carbonyl complexes wiht bridging alkylthio and diphenylarsenido ligands (μ-Ph2As)(μ-RS)Fe2(CO)6

SONG LICHENG;WANG RUJI;LI YU;WANG HONGGEN;WANG JITAO   

  • Published:1990-09-15

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379

被引次数

2

本文通过Ph2AsCl与由Fe3(CO)12, RSH, Et3N形成的盐[(μ-CO)(μ-RS)Fe2(CO)6]Et3NH作用, 制得了通式为(μ-Ph2As)(μ-RS)Fe2(CO)6五个新配合物(R=Et, Pr^n, Pr^i, Bu^n, Bu^t)。除用碳氢分析、IR及^1HNMR表征这五个配合物的结构外, 还用X光衍射技术测得R=Pr^i配合物的单晶结构。该配合物为三斜晶系, 属PI空间群晶胞参数为a=8.623(2), b=12.082(1), c=12.357(2)埃; α=84.24(1), β=71.05(1), γ=79.48(2)°; Z=2; Dx=1.62g·cm^-^3; μ=26.99cm^-^1; F(000)=584。结构分析表明, 该分子中的Fe2SAs原子构成蝶状骨架, 异丙基与骨架硫以e键相连,Fe-Fe键长为2.626埃, 它与(μ-EtS)2Fe2(CO)6, (μ-Me2P)2Fe2(CO)6及(μ-Ph2p)Fe2(CO)6的Fe-Fe键长(分别为2.537, 2.665及2.610埃)相近。

关键词: 红外分光光度法, 分子结构, 苯 P, 铁络合物, 羰基络合物, 质子磁共振谱法, 桥环化合物, 硫化合物, 砷化合物, 碳氢分析

Through the reaction of Ph2AsCl with Et3NH[(m-CO)(m-RS)Fe2(CO)6] formed from Fe3(CO)12, RSH, and Et3N, (m-Ph2As)(m-RS)Fe2(CO)6 (R = Et, Pr, CHMe2, Bu, CMe3) were prepared and characterized by elemental anal., IR and 1H NMR spectroscopy. The crystal structure of the complex with R = CHMe2 was determine by x-ray diffraction. Crystals of the complex are triclinic, space group P1, a 8.623(2), b 12.082(1), c 12.357(2) ? a 84.24(1), b 71.05(1), g 79.48(2)? Z = 2, R = 0.032, Rw = 0.042. This mol. contains a butterfly-shaped cluster skeleton Fe2SAs, to its S atom CHMe2 group is connected by an e-type of bond. The Fe-Fe bond length is 2.626 ? which is quite close to those in (m-EtS)2Fe2(CO)6(m-Me2P)2Fe2(CO)6, and (m-PhS)(m-Ph2P)Fe2(CO)6 (2.537, 2.665, and 2.610 ? resp.).

Key words: INFRARED SPECTROPHOTOMETRY, MOLECULAR STRUCTURE, BENZENE P, IRON COMPLEX, CARBONYL COMPLEX, PROTON MAGNETIC RESONANCE SPECTROMETRY, BRIDGE COMPOUNDS, SULFUR COMPOUNDS, ARSENIC COMPOUNDS

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