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出 处:《应用化学》2005年第6期615-618,共4页Chinese Journal of Applied Chemistry
基 金:国家自然科学基金(20171001;20371002);安徽省教育厅自然科学基金(2003kj251)资助项目
摘 要:合成了一种新的席夫碱配合物[NiL]ClO4(1),L为水杨醛与二乙烯三胺按1∶1摩尔比缩合的产物,晶体结构揭示在NiL+单元中Ni2+与1个O和3个N键合,配位构型近似为平面正方形。NiL+和ClO-4间的氢键相互作用没有扩展成三维结构。配合物1是抗磁性的。在N2气保护下,化合物1与K3[Fe(ox)3]·3H2O、FeSO4·7H2O按摩尔比1∶1∶1反应得配位聚合物[NiL][FeⅡFeⅢ(ox)3](2)。红外光谱结果表明,在配合物2中,FeⅡ和FeⅢ离子通过草酸根桥联形成阴离子层。变温磁化率测量结果表明,配合物2是反铁磁体,Neel温度为11K。温度高于65K,磁化率遵循CurieWeiss定律,拟合磁化率给出CurrieWeiss常数和Weiss常数的最佳值分别为10.40(2)emu·K/mol,-22.9(4)K。A new schiff-base compound, \ClO_ 4(1), was synthesized and characterized, where L represents the 1∶1 condensation product of salicylaldehyde with diethyltriamine. The crystal structure of compound 1 shows that the Ni 2+ ion in the NiL + moiety bonded with one O atom and three N atoms of the schiff-base ligand, L -, and exhibits a near square coordination geometry. The H-bonding interaction between neighboring NiL + and ClO-_ 4 ions do not form H-bonding network. The temperature dependence of magnetic susceptibility(1.8~300 K) indicates that compound 1 is diamagnetic. The compound with stoichiometry of \ \(2) was prepared by mixing the aqueous solutions of compound 1, K_ 3\·3H_ 2O and FeSO_4·7H_ 2O under N_ 2 atmosphere at ambient temperature. The IR spectrum of compound 2 illustrates that all the oxalate groups function as bridging groups, and compound 2 is actually a coordination polymer. The magnetic susceptibility measurement result at 1.8~300 K shows that this polymer possesses the anti- ferromagnetic ordering at below 11 K; the magnetic behavior above 60 K can be explained by the Curie-Weiss law, and the best fit for the magnetic susceptibility data at above 65 K gives a Curie-Weiss constant of 10.40(2) emu·K/mol and a Weiss temperature -22.9(4) K, respectively.
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