8-羟基喹啉类配体及其三角双锥钴配合物的合成与表征  

Synthesis and Characterization of 8-Hydroxyquinoline Ligand and Trigonal-bipyramidal Co(Ⅱ) Complex

作　　者：张莉艳[1] 胡逢恺[1] 黄良芳[1] 

机构地区：[1]黄山学院化学化工学院,安徽黄山245041

出　　处：《分析测试学报》2013年第4期468-472,共5页Journal of Instrumental Analysis

基　　金：安徽省高校优秀青年人才基金(2012SQRL187);黄山学院自然科学研究项目(2007xkjq015);安徽高校省级自然科学研究项目(KJ2012B178)

摘　　要：以2-甲基-8羟基喹啉作为起始原料,两步反应合成有机双齿配体HL,并通过核磁、质谱和元素分析表征其结构;配体HL与Co(NO3)2反应生成单核配合物1,该配合物属单斜晶系,P2/c空间群,晶胞参数为a=10.967(7),b=8.639(5),c=18.087(11);V=1 656.0(17)3,Z=4,Dc=1.541 mg/m3,最终R1=0.032 0,wR2=0.078 4。该配合物中钴原子是五配位,它们分别和两个配体中包含的N2O24个原子及一个吡啶N原子配位形成扭曲的三角双锥构型,X-射线粉末衍射表明其具有单一的纯相,热重分析表明其基本骨架具有较好的热稳定性。Bidentate ligand HL was prepared by two steps from the cheap commercial available 8- hydroxyquinoline and characterized by ESI - MS, NMR and elemental analysis methods. Mononucle- ar complex 1 was readily obtained in good yields by heating Co（ NO3 ）2 and HL in solution. It belongs to monoclinic system with space group P2/c, a = 10. 967（7）A, b = 8. 639（5）A, c = 18.087（ 11 ） A; V=1 656.0（17）A^3, Z=4, Dc=1.541 mg/m3, R1 =0.0320, wR2=0.0784. The cobalt atom found in the mononuclear unit is pentacoordinate, and adopts a distorted trigonal - bipyramidal geometry, and coordinates to four atoms N202 of two ligands experiment showed that the crystal structure of complex 1 was als. From TGA results, the mononuclear complex was found and one pyridine N atom. The PXRD truly representative of their bulk materi- to have a thermal stability.

关 键 词：8-羟基喹啉 合成 表征 晶体结构 

分 类 号：O657.63[理学—分析化学] O626.323[理学—化学]