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首页> 外文期刊>Journal of the Brazilian Chemical Society >Synthesis, crystal structure and thermal decomposition mechanism of a samarium o-chlorobenzoate complex with 1,10-phenanthroline
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Synthesis, crystal structure and thermal decomposition mechanism of a samarium o-chlorobenzoate complex with 1,10-phenanthroline

机译:邻氯苯甲酸sa与1,10-菲咯啉配合物的合成,晶体结构和热分解机理

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The title complex [ Sm( o-ClBA)(3)phen](2) ( o-ClBA= o-chlorobenzoate; phen= 1,10-phenanthroline) was prepared by the reaction of SmCl3 center dot 6H(2)O, o-chlorobenzoic acid and 1,10-phenanthroline. The complex was characterized by single crystal X-ray diffraction, elemental analysis, IR spectra and TG-DTG techniques. The results show that the crystal is triclinic, space group PI with a = 13.157( 3) angstrom, b = 14.139( 4) angstrom, c = 17.397( 4) angstrom, a = 83.755( 3)degrees, beta = 84.064( 3)degrees, gamma = 73.434( 3)degrees, Z= 2, Dc= 1.722 Mg/m(3), F( 000)= 1572. The crystal contains two crystallographically distinct Sm( o-ClC6H4COO)(3)( C12H8N2) units, forming two types of binuclear molecule. Each Sm3+ is coordinated to two O atoms of one bidentate chelating carboxylate group, five O atoms of two bidentate bridging and two tridentate chelating-bridging carboxylate groups, and two N atoms of one 1,10-phenanthroline molecule to complete a distorted mono-capped square antiprism geometry. Its thermal decomposition mechanism was determined by TG-DTG techniques, and kinetic parameters have been studied on the first-step decomposition of [ Sm( o-ClBA)(3) phen](2) by means of Kissinger's method and Ozawa-Doyle's method. The lifetime equation at weight-loss of 10% was deduced as ln tau = -26.8166+20319.94/T by isothermal thermogravimetric analysis.
机译:通过SmCl3中心点6H(2)O的反应制备标题复合物[Sm(o-ClBA)(3)phen](2)(o-ClBA =邻氯苯甲酸酯; phen = 1,10-菲咯啉),邻氯苯甲酸和1,10-菲咯啉。该复合物通过单晶X射线衍射,元素分析,IR光谱和TG-DTG技术表征。结果表明,晶体为三斜晶,空间群PI为a = 13.157(3)埃,b = 14.139(4)埃,c = 17.397(4)埃,a = 83.755(3)度,beta = 84.064(3 )度,γ= 73.434(3)度,Z = 2,Dc = 1.722 Mg / m(3),F(000)= 1572.晶体包含两个晶体学上不同的Sm(o-ClC6H4COO)(3)(C12H8N2)单元,形成两种类型的双核分子。每个Sm3 +与一个双齿螯合羧酸酯基团的两个O原子,两个双齿桥接和两个三齿螯合桥联羧酸酯基的五个O原子以及一个1,10-菲咯啉分子的两个N原子配位以完成一个扭曲的单封端方形反棱镜几何。通过TG-DTG技术确定了其热分解机理,并通过Kissinger法和Ozawa-Doyle法研究了[Sm(o-ClBA)(3)phen](2)第一步分解的动力学参数。 。通过等温热重分析,得出失重10%时的寿命方程为ln tau = -26.8166 + 20319.94 / T。

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