高等学校化学学报

高等学校化学学报 ›› 2005, Vol. 26 ›› Issue (3): 401.

• 研究论文 • 上一篇    下一篇

[Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O超分子化合物的晶体结构、荧光性质及热稳定性

杨锐1,2, 何水样1, 武望婷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 7500213;
    3. 聊城大学化学系,聊城252000
  • 收稿日期:2004-07-12 出版日期:2005-03-10 发布日期:2005-03-10
  • 通讯作者: 何水样(1946年出生),女,教授,主要从事稀土配位化学研究.E-mail:xdhsy@263.net E-mail:xdhsy@263.net
  • 基金资助:

    陕西省自然科学基金(批准号:2005B02);陕西省教育厅专项基金(批准号:03JK085)资助.

Crystal Structure, Fluorescence Properties and Thermal Stability of Supra-molecule Complex [Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O

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

  1. 1. Shaanxi Key Laboratory of Physico-Inorganic Chemistry, Department of Chemistry, Northwest University, Xi'an 710069, China;
    2. College of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021, China;
    3. Department of Chemistry,Liaocheng University, Liaocheng 252000, China
  • Received:2004-07-12 Online:2005-03-10 Published:2005-03-10

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摘要： 在水-乙醇混合体系中,以2-羰基丙酸水杨酰腙(C10H10N2O4,简作H3L)、1,10-菲啉C12H8N2,简作phen)与Eu(NO3)3·4H2O反应,首次培养出黄色单晶[Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O.该晶体属三斜晶系,P1空间群,晶胞参数a=1.3786(12)nm,b=1.3988(12)nm,c=1.7597(16)nm,α=73.977(11)°,β=68.598(12)°,γ=71.224(12)°,V=29.42(4)nm3,Z=2,μ=2.208mm-1,Dc=1.746Mg/m3,F(000)=1556,R=0.0377,ωR=0.0744,GOF=0.916.每个配合物晶体中均有两个相似的结构单元,每个结构单元中铕(Ⅲ)配位数为9,分别与两个2-羰基丙酸水杨酰腙和3个水分子配位;每个2-羰基丙酸水杨酰腙中的羧基氧、酰胺基中的羰基氧和CN中的氮与Eu3+配位,形成两个共边的稳定的五元环,另3个配位原子则分别来自3个水分子中的氧原子,该结构单元在空间呈扭曲的单帽四方反棱柱,而在每两个铕的九配位单元周围还有一个游离的1,10-菲啉分子和4个水分子.IR,1HNMR及热分解结果佐证了配合物的组成.该配合物具有很好的荧光特性.

关键词: 铕配合物, 2-羰基丙酸水杨酰腙, 1, 10-菲啉, 晶体结构, 荧光性质, 热分解

Abstract: A new superamolecule complex(C10H10N2O4, H3L=2-oxo-propionic acid salicyloyl hydrazone and C12H8N2=1,10-phenanthroline phen) was synthesized and its crystal structure of [Eu(C10H9N2O4)·(C10H8N2O4)(H2O)3]2·phen·4H2O was determined by X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a=1.378 6(12) nm, b=1.398 8(12) nm, c=1.759 7(16) nm, α=73.977(11)°, β=68.598(12)°, γ=71.224(12)°, V=29.42(4) nm3, Z=2, μ=2.208 mm-1, Dc=1.746 Mg/m3, F(000)=1 556, R=0.037 7, ωR=0.074 4, GOF=0.916. There are two 9-coordinated structure units in every molecule, in which Eu(Ⅲ) is coordinated by two tridentate C10H10N2O4 ligands and three water molecules and both structural units are distorted monocapped square antiprism. There are one free 1,10-phenanthrolines and four water molecules that are connected with 2-oxo-propionic acid salicyloyl hydrazone and water molecule by hydrogen bonds in the crystal cell. The complex formed a supermolecule in space through the hydrogen bonds. The composition of the complex is verified by IR, 1H NMR and thermal decomposition. The test of luminescence capacity of the complex showed that the complex has a good fluorescence.

Key words: Europium(Ⅲ) complex, 2-Oxo-propionic acid salicyloyl hydrazone, 1,10-Phenanthrolines, Crystal structure, Fluorescence property, Thermal decomposition

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