化学学报 ›› 2004, Vol. 62 ›› Issue (20): 2040-2044. 上一篇    下一篇

研究论文

镝(Ⅲ)与酰腙及1,10菲啰啉多元配合物的晶体结构及荧光性质

杨锐1,2, 何水样1, 武望婷1, 文振翼1, 史启祯1, 王大奇3   

  1. 1. 西北大学化学系, 陕西省物理无机化学重点实验室, 西安, 710069;
    2. 宁夏大学化学化工学院, 银川, 750021;
    3. 聊城大学化学系, 聊城, 252059
  • 投稿日期:2004-03-03 修回日期:2004-04-30 发布日期:2014-02-17
  • 通讯作者: 何水样,E-mail:xdhsy@263.net E-mail:xdhsy@263.net
  • 基金资助:
    陕西省自然科学基金(No.2002B05)及陕西省教育厅专项基金(No.03JK085)资助项目.

Crystal Structure, Fluorescence Characterization of Dysprosium(Ⅲ) Multicomponent Complex with Acylhydrazone and 1, 1O-Phenanthroline

YANG Rui1,2, HE Shui-Yang1, WU Wang-Ting1, WEN Zhen-Yi1, SHI Qi-Zhen1, WANG Da-Qi3   

  1. 1. Department of Chemistry, Northwest University and Shaanxi Key Laboratory of Physico-Inorganic Chemistry, Xi'an 710069;
    2. College of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021;
    3. Department of Chemistry, Liaocheng University, Liaocheng 252059
  • Received:2004-03-03 Revised:2004-04-30 Published:2014-02-17

在水乙醇混合体系中,首次得到2-羰基丙酸水杨酰腙(C10H10N2O4),1,10-菲哕啉(C12H8N2,简写作phen)与Dy(NO3)3·3H2O的配合物[Dy(C10H8N2O4)(phen)(NO3)(H2O)2]·H2O.该配合物属单斜晶系,空间群为P21/c,晶胞参数a=1.524(3)nm,b=1.1018(19)nm,c=1.468(3)nm,β=92.28(2)°,V=24.63(7)nm3,Z=4,μ=3.100 mm-1,Dc=1.831g/cm3,F(000)=1340,R=0.0314,wR=0.0660,GOF=O.966.测试结果表明,该单晶结构为镝的9配位配合物,其中一个2-羰基丙酸水杨酰腙分子以羧基氧、酰胺基中的羰基氧和C=N中的氮与Dy3+三齿配位,形成两个稳定的共边五元环,一个1,10-菲哕啉分子以二齿方式配位、一个硝酸根和两个水分子也同时参与配位,在空间呈扭曲的单帽四方反棱柱,而在配合物周围还有一个游离的水分子.发光性能测试表明配合物具有很好的荧光性能.

关键词: 镝配合物, 2-羰基丙酸水杨酰腙, 1, 10-菲啰啉, 晶体结构, 荧光性质

Dysprosium(Ⅲ) complex with 2-oxo-propionic acid salicyloyl hydrazone (C10H10N2O4) and 1,10-phenanthroline (C12H8N2, phen) has been synthesized. The yellow prismatic crystal complex crystallizes in the monoclinic system with space group P21/c and parameters a=1.524(3) nm, b=1.1018(19) nm, c=1.468(3) nm, β=92.28(2)°, V=24.63(7) nm3, Z=4, μ=3.100 mm-1, Dc=1.831 g/cm3, F(000)=1340, R=0.0314, (wR=)0.0660, GOF=0.966. Dysprosium atom is 9-coordinated by carboxyl and carbonyl O atoms and N atom of one tridentate C10H10N2O4 ligand to form two stable five-membered rings with the same edge, and the other coordinated atoms coming from one bidentate phen, one bidentate nitrate and two water molecules. The coordination polyhedron around Dy3+ was described as a monocapped square antiprism. There is a lattice water molecule in the crystal cell. Luminescence measurement shows that the complex emits fluorescence.

Key words: dysprosium(Ⅲ)complex, 2-oxo-propionic acid salicyloyl hydrazone, 1,10-phenanthroline, crystal structure, fluorescence characterization