二维Co(nip)_2(py)_2(H_2O)_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)

Hydrothermal Synthesis, Crystal Structure and Thermal Decomposition Mechanism of Two-dimensional Co(nip)_2(py)_2(H_2O)_2 Complex (nip=5-nitroisophthalate, py=pyridine)

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=1.585Mg/m3,μ(MoKα)=0.688mm-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.

The Co（nip）2（py）2（H20）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 diffraction, elemental analysis, FT-IR, DTA and TG-DTG techniques. The crystal is monoclinic, P2（1）lc 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/m^3,μ（Mo Ka） =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 decomposition mechanisms of the complex.