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化学学报
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化学学报 ›› 1995, Vol. 53 ›› Issue (8): 775-780. 上一篇    下一篇

研究论文

V-Cu-S异金属簇合物的研究I. [VS4(CuPPh3)4Br]的合成和晶体结构

余秀芬;郑发鲲   

  1. 福州大学化学系;中国科学院福建物质结构研究所;中国科学院结构化学国家重点实验室
  • 发布日期:1995-08-15

The study on the V-Cu-S heterometallic cluster I. Synthesis and Crystal structure of [VS4(CuPPh3)4Br]

YU XIUFEN;ZHENG FAKUN   

  • Published:1995-08-15

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以(NH4)3VS4为起始原料, 用低温固相法合成了标题簇合物, 并测定其晶体结构。晶体属空间群P1, 单胞参数a=1.3139(10), b=2.5113(170, c=1.1800(8)nm,α=93.04(6), β=114.86(5), γ=96.71(7)°, Z=2, μ=21.4cm^-^1, R=0.084。在簇合物中, VS4^3^-保持较严格的四面体构型, 并螯合四个Cu(I)离子连同桥Br^-离子形成具有额外面的立方烷簇骼[VS4Cu4Br]。

关键词: 晶体结构, Ｘ射线衍射分析, 溴化物, 铜络合物, 簇状化合物, 硫络合物, 钒络合物, 四硫代钒酸铵

The title compound was prepared by solid state reaction of the mixture with mole-ratio (NH4)3VS4:CuCl:PPh3:Et4NBr=1:2:3:1 at 100℃, 12 hours. The crystal structure was determined from single crystal X-ray diffraction data. It crystallizes in triclinic, space group P1, a=1.3139(10), b=2.5113(17), c=1.1800(8), α=93.04(6), β=114.86(5), γ =96.71(7)°, Z=2, μ=21.4cm^-^1, R=0.084. In the title cluster, VS4^3^- retain more serious tetrahedral configulation and chelates with for Cu(I) ions together with bridged Br^- formed a cubane with an extra face [VS4Cu4Br]core.

Key words: CRYSTAL STRUCTURE, X-RAY DIFFRACTION ANALYSIS, BROMIDE, COPPER COMPLEX, CLUSTER COMPOUND, SULFIDE COMPLEX, VANADIUM COMPLEX

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