高等学校化学学报 ›› 1990, Vol. 11 ›› Issue (10): 1045.

• 研究论文 •    下一篇

[WS4Cu2(Py)4]的合成及晶体结构

高逢君1, 朱慧珍1, 忻新泉1, 戴安邦1, 刘望喜2, 王博义2, 郑培菊2   

  1. 1. 南京大学配位化学研究所;
    2. 复旦大学测试中心
  • 收稿日期:1989-01-09 出版日期:1990-10-24 发布日期:1990-10-24
  • 通讯作者: 忻新泉, 邮编: 210008
  • 基金资助:

    联合国教科文组织;国家自然科学基金;国家教博士点基金

Synthesis and Crystal Structure of [WS4Cu2(Py)4]

Gao Fengjun1, Zhu Huizhen1, Xin Xinquan1, Dai Anbang1, Liu Wangxi2, Wang Boyi2, Zheng Peiju2   

  1. 1. Coordination Chemistry Institute, Nanjing University, Nanjing;
    2. Center of Analysis and Measurement, Fudan University, Shanghai
  • Received:1989-01-09 Online:1990-10-24 Published:1990-10-24

摘要: (NH4)2WS4、CuCl和(n-Bu)4NBr在Ar气氛中,90℃下反应10h,所得产物先后经CH2Cl2与CH3OH处理,得一桔红色晶体。该晶体与吡啶反应,即得到桔红色针状晶体[WS4Cu2(Py)4],属单斜晶系,空间群C2/c,晶胞参数:a=14.109(1)Å,b=12.704(1)Å,c=14.071(1)Å;β=96.97(1)°;Z=4。结构用重原子法解出,经最小二乘法修正,偏离因子R=0.027。

关键词: 硫代钨酸盐, 固相反应, 簇合物

Abstract: The reaction among (NH4)2WS4, CuCl and (n-Bu)4NBr yields red-orange crystal. The Crystal reacts with excess of pyridine to produce red-orange crystal [WS4Cu2(Py)4]. It belongs to the monoclinic system, space group C2/c,with a=14.109(1)Å, 6=12. 704(1)Å, c=14. 071(1)Å; β=96. 97(1)°; V=2504.1Å3 and Z=4. The intensity data were collected by ENRAF-NONIUS CAD4 diffractometer. The molecular structure was solved by patterson method and Fourier method and refined by least-squres with anisotropic thermal parameters. The value of Ris 0.027.

Key words: Thiotungstates, Solid state reaction, Cluster

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