高等学校化学学报

高等学校化学学报

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含有十二元环交叉孔道的新颖亚磷酸铟[In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O)的水热合成与表征

刘成站1,2, 朱广山1, 金钊1, 薛铭1, 孙福兴1, 方千荣1, 裘式纶1   

    1. 吉林大学化学学院, 无机合成与制备化学国家重点实验室, 长春 130012;
    2. 东北师范大学化学学院, 长春 130024
  • 收稿日期:2007-01-11 修回日期:1900-01-01 出版日期:2007-10-10 发布日期:2007-10-10
  • 通讯作者: 裘式纶

Hydrothermal Synthesis and Characterization of a New Indium Phosphite [In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O) with Intersectin

LIU Cheng-Zhan1,2, ZHU Guang-Shan1, JIN Zhao1, XUE Ming1, SUN Fu-Xing1, FANG Qiang-Rong1, QIU Shi-Lun1*   

    1. State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, China;
    2. School of Chemistry, Northeast Normal University, Changchun 130024, China
  • Received:2007-01-11 Revised:1900-01-01 Online:2007-10-10 Published:2007-10-10
  • Contact: QIU Shi-Lun

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摘要： 在含有HF的体系中, 用乙二胺作模板剂, 通过水热方法合成了一个新的三维亚磷酸铟[In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O), 并对其进行了红外光谱、热重、ICP和CHN元素分析等表征. 单晶X射线衍射分析结果表明, 该化合物属于三方晶系, P3空间群, 晶胞参数a=1.37883(7) nm, c=0.93450(9) nm, V=1.53862(2) nm3, Z=2, Dc=2.489 Mg/m3, 最终一致性因子R1[I >2σ(I)]=0.0526, wR2[I>2σ(I)]=0.1328, GOF=1.082. 其结构中的InO6八面体、InO5(H2O)八面体和HPO3假四面体通过O原子共顶点连接, 分别沿a, b轴方向形成含有十二元环的交叉孔道, 客体水分子和双质子化的乙二胺分子存在于孔道中.

关键词: 水热合成, 晶体结构, 乙二胺, 亚磷酸铟

Abstract: A new three-dimensional indium phosphite, [In4(HPO3)7(H2O)3](NH3CH2CH2NH3)·(H2O), was synthesized under hydrothermal conditions in the system containing HF using ethylenediamine as the template and characterized by IR spectroscopy, TG, ICP and C, H, N elemental analysis. The result of single-crystal X-ray diffraction analysis reveals that the title compound crystallized in trigonal system, space group P3 with unit cell parameters a=1.37883(7) nm, c=0.93450(9) nm, V=1.53862(2) nm3, Z=2, Dc=2.489 Mg/m3, R1[I>2σ(I)]=0.0526, wR2[I>2σ(I)]=0.1328, GOF=1.082. Its structure is built up from shared vertex linking InO6, InO5(H2O) octahedral and HPO3 pseudo-pyramidal units by O atoms, forming intersecting twelve-membered ring channels along a and b axes directions. Guest water and diprontonated ethylenediamine molecules exist in the channels.

Key words: Hydrothermal synthesis, Crystal structure, Ethylenediamine, Indium phosphite

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