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化学学报
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化学学报 ›› 2004, Vol. 62 ›› Issue (4): 391-398. 上一篇    下一篇

研究论文

多钒硼酸盐H3{[Cu(en)2]5[(VO)12O6B18O42]}[B(OH)3]2·16H2O的水热合成、晶体结构和性质

林志华1, 张汉辉1,2, 黄长沧1,2, 孙瑞卿1, 陈义平1, 吴小园1   

  1. 1. 福州大学化学系, 福州, 350002;
    2. 中国科学院福建物质结构研究所结构化学国家重点实验室, 福州, 350002
  • 投稿日期:2003-04-08 修回日期:2003-10-13 发布日期:2014-01-26
  • 通讯作者: 张汉辉,E-mail:hhzhang@fzu.edu.cn E-mail:hhzhang@fzu.edu.cn
  • 基金资助:
    福建省自然科学基金(No.E0110013)、福建省科技三项基金(No.K02028)和结构化学国家重点实验室资助项目.

Hydrothermal Synthesis, Crystal Structure and Properties of Polyoxovanadium Borate H3{[Cu(en)2]5[(VO)12O6B18O42]}[B(OH)3<>/sub]2·16H2O

LIN Zhi-Hua1, ZHANG Han-Hui1,2, HUANG Chang-Cang1,2, SUN Rui-Qing1, CHEN Yi-Ping1, WU Xiao-Yuan1   

  1. 1. Department of Chemistry, Fuzhou University, Fuzhou 350002;
    2. State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002
  • Received:2003-04-08 Revised:2003-10-13 Published:2014-01-26

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用H3BO3, NH4VO3, Cu(CH3COO)2·H2O和乙二胺在水热条件下合成了新颖结构的多钒硼酸盐H3{[Cu(en)2]5-[(VO)12O6B18O42]}[B(OH)3]2·16H2O,对其进行了单晶X射线衍射、红外光谱、拉曼光谱、紫外-可见漫反射光谱、荧光光谱、顺磁共振谱和热重分析表征.在该化合物的结构中,环状的B18O42通过18个B-(μ3-O)-V键被两个V6O18簇夹在中间,簇阴离子[(VO)12O6B18O42]13-分别通过4个[Cu(en)2]2+与邻近的簇阴离子靠静电相互作用连接成无限二维网状结构,其空洞尺寸为0.619～1.817 nm.

关键词: 水热合成, 多钒硼酸盐, 晶体结构, 簇合物

350002) A novel polyoxovanadium borate H3{[Cu(en)2]5[(VO)12O6B18O42]}[B(OH)3]2 has been synthesized from a mixture of H3BO3, NH4VO3, Cu(CH3COO)2·H2O and ethylenediamine under hydrothermal condition and characterized by crystal X-ray structure analysis, IR spectrum, Raman spectrum, UV-Vis DRIS spectrum, fluorescence spectrum,ESR and TGA. In the structure of the compound, there is a ring of B18O42 sandwiched between two vanadium oxygen clusters V6O18 by eighteen B—(μ3O)—V bonds, and the anion clusters [(VO)12O6B18O42]13- are connected through four [Cu(en)2]2+ by the static electronic interaction. Thus, the complex was extended to an infinite two dimensional network structure, with size of the hole amounting to 0.619～1 817 nm.

Key words: hydrothermal synthesis, polyoxovanadium borate, crystal structure, cluster compound