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3,4-二甲氧基苯乙酸邻菲咯啉轻稀土配合物的合成、晶体结构、荧光光谱及热行为
引用本文:余玉叶,李花琼,刘建风,赵国良.3,4-二甲氧基苯乙酸邻菲咯啉轻稀土配合物的合成、晶体结构、荧光光谱及热行为[J].无机化学学报,2010,26(12):2266-2272.
作者姓名:余玉叶  李花琼  刘建风  赵国良
作者单位:1. 浙江师范大学化学与生命科学学院,金华,321004;金华职业技术学院,金华,321007
2. 浙江师范大学化学与生命科学学院,金华,321004
3. 浙江师范大学化学与生命科学学院,金华,321004;浙江师范大学行知学院,金华,321004
摘    要:合成了3,4-二甲氧基苯乙酸邻菲咯啉轻稀土配合物:RE2(DMPA)6(phen)2](RE=Ce (1),Pr (2),Nd (3),Eu (4);HDMPA=3,4-二甲氧基苯乙酸,C12H12O4;phen=1,10-邻菲咯啉),用元素分析、红外光谱、热重分析对产物进行表征,用单晶X-射线衍射方法测定了配合物3的晶体结构。配合物C84H82Nd2N4O24 (3)属于三斜晶系,P1 空间群,晶胞参数:a=1.242 06(9) nm,b=1.244 56(9) nm,c=1.477 88(11) nm,α=90.617(4)°,β=103.486(4)°,γ=116.870(3)°,晶胞体积:V=1.963 8(2) nm3,晶胞内结构基元数Z=1,分子量Mr=1 820.02,电子数F(000)=926,密度Dc=1.539 g·cm-3,吸收系数μ(Mo Kα)=1.389 mm-1。测定了铕配合物的荧光光谱,荧光光谱表明,配合物显示了铕(Ⅲ)离子的特征发射,这表明配体将吸收的能量有效地转移给了中心离子,配体起到了很好的敏化作用。同时也测定了铕配合物的热分解情况,并利用TG-DTG曲线采用非等温积分法和微分法研究了热分解动力学机理。

关 键 词:稀土配合物    3,4-二甲氧基苯乙酸    邻菲咯啉    晶体结构    荧光光谱    热分解动力学机理

Synthesis, Crystal Structure, Luminescence Spectrum and Thermal Analysis of Light Rare Earth Complexes from 3,4-Dimethoxyphenylacetic Acid and 1,10-Phenanthroline
YU Yu-Ye,LI Hua-Qiong,LIU Jian-Feng and ZHAO Guo-Liang.Synthesis, Crystal Structure, Luminescence Spectrum and Thermal Analysis of Light Rare Earth Complexes from 3,4-Dimethoxyphenylacetic Acid and 1,10-Phenanthroline[J].Chinese Journal of Inorganic Chemistry,2010,26(12):2266-2272.
Authors:YU Yu-Ye  LI Hua-Qiong  LIU Jian-Feng and ZHAO Guo-Liang
Institution:College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua, Zhejiang 321004; Jinhua College of Occupation and Technology, Jinhua, Zhejiang 321007,College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua, Zhejiang 321004,College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua, Zhejiang 321004 and College of Chemistry and Life Sciences, Zhejiang Normal University, Jinhua, Zhejiang 321004; Zhejiang Normal University Xingzhi College, Jinhua, Zhejiang 321004
Abstract:Four light rare earth coordination polymers RE2(DMPA)6(phen)2] (RE=Ce (1), Pr (2), Nd (3), Eu (4);HDMPA=3,4-dimethoxyphenylaoetic acid, C12H12O4; phen=1,10-phenanthroline) were synthesized and characterized by elemental analysis, IR, TG-DTG and X-ray crystallographically. The single-crystal X-ray diffraction studies demonstrated that complex 3 is formed 3D supramolecular architectures by hydrogen bonds and Π-Π stacking interactions. In all these complexes, the coordination number around REOID center is nine. The fluorescence spectrum of complex 4 is investigated. It is indicated that the luminescence behavior of complex results from metalcentered emission, ligand can transfer the energy to the central metal efficiently and can sensitize the central metal. The thermal decomposition of complex 4 and its kinetic mechanisms and equations are studied under the nonisothermal integral and differential methods in air by TG-DTG curves. CCDC: 732322, 3.
Keywords:rare earth complex  3  4-dimethoxyphenylacetic acid  1  10-phenanthroline  crystal structure  fluorescence spectrum  kinetic mechanism of thermal decomposition
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