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化学学报
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化学学报 ›› 2010, Vol. 68 ›› Issue (21): 2206-2210. 上一篇    下一篇

研究论文

铜-有机多酸配合物[CuI(2,2 -bipy)2]{[CuII(2,2 -bipy)2]2(BW12O40)}•4H2O的原位合成、晶体结构与表征

赵胜能1，邵学义1，王志花1，靳素荣*,1，孟祥高2   

  1. (1武汉理工大学理学院化学系 武汉 430070)
    (2华中师范大学化学学院 武汉 430072)
  • 投稿日期:2010-02-20 修回日期:2010-07-05 发布日期:2010-07-05
  • 通讯作者: 靳素荣 E-mail:rsjin@whut.edu.cn
  • 基金资助:

    无机－有机杂化材料的水热合成、结构与性质研究

In-situ Synthesis, Crystal Structure and Characterization of Copper- organic Polyacid Complex [CuI(2,2 -bipy)2]{[CuII(2,2 -bipy)2]2- (BW12O40)}•4H2O

Zhao Shengneng1 Shao Xueyi1 Wang Zhihua1 Jin Surong*,1 Meng Xianggao2   

  1. (1 School of Science, Wuhan University of Technology, Wuhan 430070)
    (2 College of Chemistry, Central China Normal University, Wuhan 430072)
  • Received:2010-02-20 Revised:2010-07-05 Published:2010-07-05

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在水热条件下, K5BW12O4•nH2O, CuSO4•5H2O, 2,2 -联吡啶-3,3 -二羧酸在水溶液中进行原位反应, 得到一维链状化合物[CuI(2,2 -bipy)2]{[CuII(2,2 -bipy)2]2(BW12O40)}•4H2O, 并对其进行了元素分析, IR, TG, CV和单晶X射线衍射表征. 结果表明, 化合物属于单斜晶系, P21/n空间群, 晶胞参数a＝1.88365(14) nm, b＝2.04178(15) nm, c＝2.16724(16) nm, α＝90°, β＝96.6720(10)°, γ＝90°, V＝8.2786(11) nm3, Z＝4, Dc＝3.255 g/cm3, R1＝0.0575, wR2＝0.1073. 化合物分子结构单元由1个铜-有机多酸阴离子{[CuII(2,2 -bipy)2]2(BW12O40)}－, 1个配位阳离子[CuI(2,2 -bipy)2]＋, 4个结晶水分子构成. 化合物分子通过氢键和π-π堆积作用形成二维超分子体系. 电化学研究表明, 化合物存在三步氧化还原过程.

关键词: 铜-有机多酸配合物, 多金属氧酸盐, 原位合成, 晶体结构

A novel copper-organic polyacid complex [CuI(2,2 -bipy)2]{[CuII(2,2 -bipy)2]2(BW12O40)}•4H2O was synthesized by in-situ generation of 2,2 -bipyridine from 2,2 -bipyridine-3,3 -dicarboxylate precursor under hydrothermal condition and characterized by elemental analysis, IR, TG, CV and single-crystal X-ray diffraction. The title compound crystallized in a monoclinic crystal system, with space group P21/n, a＝1.88365(14) nm, b＝2.04178(15) nm, c＝2.16724(16) nm, α＝90°, β＝96.6720(10)°, γ＝90°, V＝8.2786(11) nm3, Z＝4, Dc＝3.255 g/cm3, R1＝0.0575, wR2＝0.1073. The compound consists of copper-organic polyoxoanion {[CuII(2,2 -bipy)2]2(BW12O40)}－, cations [CuI(2,2 -bipy)2]＋, lattice water molecules and formed a 2D supramolecular networks by hydrogen bond and π-π stacking of 2,2 -bipyridine. The cyclic voltammogram indicated that three couples redox waves were observed on the compound modified carbon paste electrode (1-CPE).

Key words: copper-organic polyacid complex, polyoxometalate, in-situ synthesis, crystal structure