溶剂诱导的两例单核Er3+配合物的合成、晶体结构及磁性  

Solvent-Induced Syntheses,Crystal Structures and Magnetic Properties of Two Mononuclear Er(Ⅲ)Complexes

作　　者：郗婧 麻秀芳 徐燕红 周惠良 周钰婷 刘翔宇 XI Jing;MA Xiu-Fang;XU Yan-Hong;ZHOU Hui-Liang;ZHOU Yu-Ting;LIU Xiang-Yu(State Key Laboratory of High-Efficiency Coal Utilization and Green Chemical Engineering,National Demonstration Center for Experimental Chemistry Education,College of Chemistry and Chemical Engineering,Ningxia University,Yinchuan 750021,China)

机构地区：[1]宁夏大学化学化工学院,煤炭高效利用与绿色化工国家重点实验室,国家级实验教学示范中心,银川750021

出　　处：《无机化学学报》2020年第5期927-932,共6页Chinese Journal of Inorganic Chemistry

基　　金：国家自然科学基金(No.21863009,21463020);宁夏回族自治区国内一流学科建设项目(No.NXYLXK2017A04);宁夏回族自治区大学生创新创业训练计划(No.2019107490041)资助。

摘　　要：通过调整溶剂组分的比例,成功合成了2例结构不同的单核Er3+配合物:[Er(bpad)3]·CH3OH·H2O(1)和[Er(bpad)2(H2O)2]NO3·3H2O(2)(Hbpad=N^3-苯甲酰吡啶基-2-羰基氨基酰腙)。在甲醇/水(2:1,V/V)的混合溶剂中加入Er(NO3)3·6H2O、Hbpad和三乙胺反应制得黄色晶体配合物1。配合物2的合成方法与1相似,仅将溶剂组分甲醇和水的体积比调整为1:2。通过红外光谱、元素分析对2例配合物进行了表征。2例配合物在空气中都有良好的稳定性,并在室温下均保持晶体的完整性。晶体结构分析表明,配合物1和2中的Er^3+金属中心分别显示了九配位和八配位环境。配合物1中Er^3+离子表现为单帽四方反棱柱构型,而配合物2中Er^3+离子呈现了双帽三棱柱构型。此外,2例配合物的直流和交流磁化率测试结果表明,1和2在零场下均未展示出单分子磁体特征。By adjusting the ratio of the solvent components,two mononuclear erbium complexes,[Er(bpad)3]·CH3 OH·H2 O(1)and[Er(bpad)2(H2 O)2]NO3·3 H2 O(2)(Hbpad=N3-benzoylpyridine-2-carboxamidrazone),have been successfully synthesized.In the mixure of methanol and water solvent(2:1,V/V),yellow crystals of 1 were prepared by solution reaction of Er(NO3)3·6 H2 O,Hbpad and triethylamine.Interestingly,complex 2 was obtained by the similar way of 1,while the volume ratio of CH3 OH to H20 is altered to be 1:2.The resulting complexes were characterized by IR spectrum,elemental analysis.Two complexes are air stable,and can maintain the crystalline integrities at ambient conditions.Crystal structure analysis indicates that the Er(Ⅲ)ions in 1 and 2 present nonacoordinated and octa-coordinated environments in different coordination geometries,respectively.Monocapped square antiprism(C4 v)is formed in 1,while biaugmented trigonal prism(C2 v)is observed in 2.The direct-current(dc)and alternating-current(ac)magnetic susceptibilities of 1 and 2 have been analyzed as well.CCDC:1478582,1;1478579,2.

关 键 词：铒配合物 溶剂效应 晶体结构 磁性 

分 类 号：O614.344[理学—无机化学]