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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=1.24206(9)nm,b=1.24456(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,配合物显示了铕髥离子的特征发射,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。
Synthesis of 3,4-dimethoxyphenylacetic acid phenanthroline light rare earth complexes: [RE2 (DMPA) 6 (phen) 2] (RE = Ce Eu (4); HDMPA = 3,4-dimethoxyphenylacetic acid, C12H12O4; phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, The crystal structure of complex 3 was determined by X-ray diffraction. The complex C84H82Nd2N4O24 (3) belongs to the triclinic system with space group P1 and unit cell parameters of a = 1.24206 (9) nm, b = 1.24456 (9) nm, c = 1.47788 ) =, Β = 103.486 (4) °, γ = 116.870 (3) °, the unit cell volume is V = 1.963 8 (2) nm3, the unit cell number is Z = 1, the molecular weight is Mr = 8202.02, The number F (000) = 926, the density Dc = 1.539 g.cm-3, the absorption coefficient μ (Mo Kα) = 1.389 mm-1. The fluorescence spectra of europium complexes were determined. The fluorescence spectra showed that the complexes showed the characteristic emission of europium ions, indicating that the ligand efficiently transfers the absorbed energy to the central ion and the ligand plays a good sensitizing effect . At the same time, the thermal decomposition of europium complex was also measured. The kinetic mechanism of thermal decomposition was also studied by TG-DTG curve using non-isothermal integration method and differential method.