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化学学报
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化学学报 ›› 2006, Vol. 64 ›› Issue (16): 1693-1699. 上一篇    下一篇

研究论文

二维Co(nip)2(py)2(H2O)2配合物的水热合成, 晶体结构和热分解机理研究(nip＝5-硝基间苯二甲酸根, py＝吡啶)

郭金玉, 张建国, 张同来*   

  1. (北京理工大学爆炸科学与技术国家重点实验室 北京 100081)
  • 投稿日期:2005-12-05 修回日期:2006-02-20 发布日期:2006-08-28
  • 通讯作者: 张同来*

Hydrothermal Synthesis, Crystal Structure and Thermal Decomposi-tion Mechanism of Two-dimensional Co(nip)2(py)2(H2O)2 Complex (nip＝5-nitroisophthalate, py＝pyridine)

GUO Jin-Yu; ZHANG Jian-Guo; ZHANG Tong-Lai*   

  1. (State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081)
  • Received:2005-12-05 Revised:2006-02-20 Published:2006-08-28
  • Contact: ZHANG Tong-Lai

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用水热法以5-硝基间苯二甲酸和吡啶为配体合成并培养了Co(nip)2(py)2(H2O)2的单晶. 对单晶进行了X射线单晶衍射分析、元素分析、傅里叶变换红外光谱分析、差热分析和热重-微商热重分析. 该配合物晶体为单斜晶系, 属于P2(1)/c空间群. 晶胞参数为a＝1.1662(3) nm, b＝1.7734(4) nm, c＝0.6988(2) nm, β＝102.46(4)°, V＝1.4112(6) nm3, Z＝2, Dc＝1.585 Mg/m3, μ(Mo Kα)＝0.688 mm－1. 所有晶体数据的R因子为: R1＝0.1064, wR2＝0.1270; 最终R因子[I＞2σ(I)]为: R1＝0.0467, wR2＝0.1008. X射线单晶衍射分析的结果表明, 依靠分子内氢键、分子间氢键、硝基氧之间的弱相互作用以及π-π堆积作用, 配合物分子被连成二维无限平面结构. 根据配合物的热分析结果, 配合物及热分析各阶段残渣的傅里叶变换红外光谱, 我们推测出了配合物的热分解机理.

关键词: 晶体结构, 5-硝基间苯二甲酸, 吡啶, 热分解机理

The Co(nip)2(py)2(H2O)2 crystal (nip＝5-nitroisophthalate, py＝pyridine) was synthesized and cultured by hydrothermal method using 5-nitroisophthalic acid and pyridine as ligands. The crystal was characterized by X-ray single crystal diffrac-tion, elemental analysis, FT-IR, DTA and TG-DTG techniques. The crystal is monoclinic, P2(1)/c space group, with parameters of a＝1.1662(3) nm, b＝1.7734(4) nm, c＝0.6988(2) nm, β＝102.46(4)°, V＝1.4112(6) nm3, Z＝2, Dc＝1.585 Mg/m3, μ(Mo Kα)＝0.688 mm－1. R indices for all data are R1＝0.1064, wR2＝0.1270; the final R indices [I＞2σ(I)] are R1＝0.0467, wR2＝0.1008. The X-ray single crystal diffraction analysis demonstrates that the molecules of the coordination compound are linked to form two-dimensional frameworks by means of intra- and intermolecular hydrogen bonds, the weak interactions between O atoms of NO2 and π-π stacking interactions. According to the thermal analyses and FT-IR spectra, we got the possible thermal de-composition mechanisms of the complex.

Key words: crystal structure, 5-nitroisophthalic acid, pyridine, thermal decomposition