高等学校化学学报 ›› 2001, Vol. 22 ›› Issue (4): 535.

• 研究论文 • 上一篇    下一篇

稀土-反式-2,3-二甲基丙烯酸-邻菲咯啉混配配合物的合成与表征

陆维敏, 吴斌, 汪丽娜   

  1. 浙江大学催化研究所, 杭州 310028
  • 收稿日期:1999-08-02 出版日期:2001-04-24 发布日期:2001-04-24
  • 通讯作者: 陆维敏(1951年出生),男,硕士,教授,从事催化和配位化学研究.
  • 基金资助:

    浙江省教育委员会资助

Synthesis and Characterization of Bis(1,10-phenanthroline) tri(trans-2,3-dimethylacrylato) Lanthanide(Ⅲ) Dinuclear Complexes

LU Wei-Min, WU Bin, WANG Li-Na   

  1. Institute of Catalysis, Zhejiang University, Hangzhou 310028, China
  • Received:1999-08-02 Online:2001-04-24 Published:2001-04-24

摘要: 合成了一种新的双核稀土配合物[REL3(phen)]2(RE=La,Ce,Pr,Nd,Sm,Eu,L=反式CH3CHC(CH3)COO-,phen=phenanthroline),并且用红外光谱、紫外光谱、核磁共振谱和元素分析等进行了表征,其中测定了[LaL3phen]2的晶体结构.晶体属单斜晶系,P21/n空间群,Z=2,晶胞参数a=1.2962(4)nm,b=1.3283(4)nm,c=1.5485(5)nm,β=95.45(2)°,最终偏差因子R=0.033,RW=0.040.配合物分子为一个中心对称的双核分子,镧离子由两个双齿羧基和两个μ2-O羧基桥联,La…La*距离为0.4094nm.中心离子为九配位,形成畸变的三帽三棱柱配位多面体.La—O和La—N的键长范围分别为0.2460~0.2756nm和0.2718~0.2760nm.

关键词: 稀土, 反式-2, 3-二甲基丙烯酸, 邻菲咯啉, 晶体结构

Abstract: Novel dinuclear lanthanide complexes, [REL3(phen)]2(RE=La, Ce, Pr, Nd, Sm, Eu; L=trans-2,3-dimethylacrylate, phen=phenanthroline), have been synthesized and characterized by IR, NMR, UVspectroscopy and elemental analysis. The single crystal of [LaL3phen]2 has been determined by X-ray crystallography, which crystallizes in the monoclinic, space group P2 1/n with Z=2, cell dimensions a=1.2962(4) nm, b=1.3283(4) nm, c=1.5485(5) nm, β=95.45(2)°. The structure was refined to R=0.033 for observed 3112 reflections and consists of centrosymmetric dinuclear molecule. Lanthanum atoms are bridged by two bidenate and two terdentate carboxylato groups with La…La separation of 0.4094 nm. Each Lanthanum atom is nine coordinate and exhibits a distorted tricapped trigonal prism. The La—Oand La—Nbond distances are in the range of 0.2460 —0.2756 and 0.2718—0.2760 nm, respectively.

Key words: Rare earth metal, trans-2,3-Dimethylacrylic acid, 1,10-Phenanthroline, Crystal structure

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