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化学学报
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化学学报 ›› 2006, Vol. 64 ›› Issue (5): 371-374. 上一篇    下一篇

研究论文

微孔[Me4N]2HgGe4S10的溶剂热合成与表征

朱阳春1，白音孟和1，刘新1，贾翠英1，刘晓阳2，安永林*,1   

  1. (1大连理工大学化学系 大连116024)
    (2吉林大学无机合成与制备国家重点实验室 长春130012)
  • 投稿日期:2005-05-18 修回日期:2005-11-07 发布日期:2006-03-15
  • 通讯作者: 安永林

Solvothermal Synthesis and Characterization of an Open-Framework [Me4N]2HgGe4S10

ZHU Yang-Chun1, BAIYIN Meng-He1, LIU Xin1, JIA Cui-Ying1, LIU Xiao-Yang2, AN Yong-Lin*,1   

  1. (1 Department of Chemistry, Dalian University of Technology, Dalian 116024)
    (2 Key Laboratory of Inorganic Synthesis and Preparation, Jilin University, Changchun 130012)
  • Received:2005-05-18 Revised:2005-11-07 Published:2006-03-15
  • Contact: AN Yong-Lin

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用溶剂热方法合成了[Me4N]2HgGe4S10, 通过单晶X射线衍射, IR, DSC-TG手段对其进行了表征. 结果表明, 标题化合物属四方晶系, I-4空间群, 晶胞参数a＝0.92687(8) nm, c＝1.43739(12) nm, V＝1.23484(18) nm3, Z＝2, Mo Kα λ＝0.071073 nm, R1＝0.0570, wR2＝0.1374, 空旷骨架结构由超四面体Ge4S10与HgS4四面体共用顶点连接而成, 有机模板离子在一维孔道中. 该化合物具有一定的热稳定性, 在320 ℃发生分解形成GeS2.

关键词: 溶剂热合成, 晶体结构, 开放骨架, 热稳定性

An open-framework [Me4N]2HgGe4S10 (1) was solvothermally synthesized and characterized by single crystal diffraction, IR and DSC-TG techniques. Compound 1 was built up from supertetrahedra and HgS4, and has 1D channels with pore sizes of 0.94 nm×0.65 nm along direction a or b. TG-DSC results indicated that 1 has a good thermal stability in a nitrogen. Crystal data for 1: Mr＝957.55, space group I-4, a＝0.92687(8) nm, c＝1.43739(12) nm, V＝1.23484(18) nm3, Z＝2, Mo Kα λ＝0.071073 nm, R1＝0.057, wR2＝0.1374 for 906 reflections with I＞2σ(I).

Key words: solvothermal synthesis, crystal structure, open-framework, thermal stability