高等学校化学学报

高等学校化学学报 ›› 2002, Vol. 23 ›› Issue (9): 1641.

• 研究论文 •    下一篇

[(η5-C5Me5)WS3Cu3Br2(PPyPh2)2]四核簇合物的合成和晶体结构

徐庆锋, 陈金香, 刘泉, 纪顺俊, 郎建平, 沈琪   

  1. 苏州大学化学化工系, 苏州 215006
  • 收稿日期:2002-01-06 出版日期:2002-09-24 发布日期:2002-09-24
  • 通讯作者: 郎建平(1964年出生),男,博士,教授,博士生导师,从事金属有机化学研究.E-mail:jplang@suda.edu.cn E-mail:jplang@suda.edu.cn
  • 基金资助:

    江苏省有机化学重点实验室开放基金(批准号:T5109002);苏州大学人才引进基金(批准号:XQ109020)资助

Synthesis and Crystal Structure of a Tetranuclear Cluster [(η5-C5Me5)WS3Cu3Br2(PPyPh2)2]

XU Qing-Feng, CHEN Jin-Xiang, LIU Quan, JI Shun-Jun, LANG Jian-Ping, SHEN Qi   

  1. Department of Chemistry and Chemical Engineering, Suzhou University, Suzhou 215006, China
  • Received:2002-01-06 Online:2002-09-24 Published:2002-09-24

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摘要： 以[PPh4]2[(η5-C5Me5)WS3(CuBr)3]2和diphenyl-2-pyridylphosphine(PPyPh2)在乙腈中反应得到标题化合物[(η5-C5Me5)WS3Cu3Br2(PPyPh2)2],对该产物进行了元素分析、IR、UV-Vis和1H NMR谱表征,并测定了晶体结构.该化合物晶体属三斜晶系,P1空间群,晶胞参数:a=1.5459(7)nm,b=1.620(1)nm,c=1.0180(2)nm,α=94.18(3)°,β=97.38(3)°,γ=111.81(4)°,V=2.327(2)nm3,Z=2,Dc=1.84g·nm-3,F(000)=1260,μ=57.77cm-1,最终偏离因子R=0.029.此簇合物结构可视为由一个[(η5-C5Me5)WS3]单元和3个Cu组成的开口立方烷,其中2个Cu是畸变四面体配位,第3个Cu是近似三角平面配位.W—Cu(1),W—Cu(2)和W—Cu(3)距离分别为0.27041(9),0.27327(8),0.26785(9)nm.

关键词: 钨簇合物, 铜簇合物, 硫簇合物, 晶体结构

Abstract: Reaction of [PPH4]2[(η5-C5Me5)WS3(CuBr)3]2 in CH3CN with PPyPh2 in a molar ratio of 1∶4 gave rise to red crystals of [(η5-C5Me5)WS3Cu3Br2(PPyPh2)2]. It was characterized by elemental analysis, IR, UV-Vis and 1H NMR spectroscopy and X-ray diffraction. It crystallizes in a triclinic system with space group P1 and unit cell parameters a=1.5459(7) nm, b=1.620(1) nm, c=1.0180(2) nm, α=94.18(3)°, β=97.38(3)°, γ=111.8(4)°, Z=2, R=0.031. The structure consists of a distorted WS3Cu3Br cubane where the Cu(3)—Br(1) bond is broken. Cu(1) and Cu(2) atoms adopt a distorted tetrahedral geometry coordination while Cu(3) assumes an approximately trigonal planar geometry. W—Cu(1), W—Cu(2) and W—Cu(3) distances are 0.27041(9), 0.27327(8), and 0.26785(9) nm, respectively.

Key words: Tungsten cluster, Copper cluster, Sulfide cluster, Crystal structure

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