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化学学报
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化学学报 ›› 2008, Vol. 66 ›› Issue (17): 2011-2016. 上一篇    

研究简报

混合价配位聚合物 - [Cu(en)2H2O]2•8H2O的水热合成与晶体结构

靳素荣*,a 张联盟b 柳士忠c 孟祥高d

  

  1. (a武汉理工大学理学院化学系 武汉 430070)
    (b武汉理工大学材料复合新技术国家重点实验室 武汉 430070)
    (c湖北大学化学化工学院 武汉 430062)
    (d华中师范大学化学学院 武汉 430072)

  • 投稿日期:2008-04-23 修回日期:2008-06-25 发布日期:2008-09-14
  • 通讯作者: 靳素荣

Hydrothermal Synthesis and Crystal Structure of a Mixed-valence Coordination Polymer - [Cu(en)2H2O]2•8H2O

JIN, Su-Rong *,a ZHANG, Lian-Meng b LIU, Shi-Zhong c MENG, Xiang-Gao d   

  1. (a School of Science, Wuhan University of Technology, Wuhan 430070)
    (b State Key Laboratory of Advanced Technology for Materials Synthesis and Processing,
    Wuhan University of Technology, Wuhan 430070)
    (c School of Chemistry and Chemical Engineering, Hubei University, Wuhan 430062)
    (d College of Chemistry, Central China Normal University, Wuhan 430072)
  • Received:2008-04-23 Revised:2008-06-25 Published:2008-09-14
  • Contact: JIN, Su-Rong

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在水热条件下合成了一个新的混合价配位聚合物 [Cu(en)2H2O]2•8H2O, 并对其进行了元素分析, IR, UV, TG-DSC等表征. X射线单晶衍射结果表明, 化合物属于单斜晶系, P21/c空间群, 晶胞参数a＝1.88678(12) nm, b＝2.30383(14) nm, c＝2.61234(16) nm, α＝90°, β＝95.844(1)°, γ＝90°, V＝11.2964(12) nm3, Z＝4, Dc＝3.954 g/cm3, R1＝0.0975, wR2＝0.2041. 结构测定结果表明, 聚合物中杂多阴离子骨架通过氧桥相连并形成一维无限链. 热性质研究表明, 形成标题化合物后杂多阴离子骨架分解温度大约在600.4 ℃, 热稳定性较母体杂多酸明显增强.

关键词: 水热合成, 晶体结构, 多金属氧酸盐, 混合价, Keggin结构

A novel mixed-valence coordination polymer [Cu(en)2H2O]2• 8H2O was synthesiszed under a hydrothermal condition and characterized by elemental analysis, IR, UV, TG-DSC and single-crystal X-ray diffraction. The title compound crystllized in a monoclinic crystal system, with space group P21/c, a＝1.88678(12) nm, b＝2.30383(14) nm, c＝2.61234(16) nm, α＝90°, β＝95.844(1)°, γ＝90°, V＝11.2964(12) nm3, Z＝4, Dc＝3.954 g/cm3, R1＝0.0975, and wR2＝0.2041. The structural refinement indicates that the title compound forms a one-dimensional chain from the polyanions ( )6－ through O bridge. The result of TG-DSC shows that the title compound is thermally more stable than α-H3PW12O40•H2O.

Key words: hydrothermal synthesis, crystal structure, polyoxometallate, mixed-valence, Keggin structure