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化学学报
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化学学报 ›› 2007, Vol. 65 ›› Issue (16): 1588-1592. 上一篇    下一篇

研究论文

一个新颖的三维异核锑(III)-镨(III)配合物[Sb2-μ4-(EDTA)2Pr(H2O)5]NO3•4H2O的合成、晶体结构及热分解研究

沈娟1, 蒋琪英1, 钟国清*,1, 贾玉庆2, 郁开北3   

  1. (1西南科技大学化学系 绵阳 621010)
    (2华东理工大学化学系 上海 200237)
    (3中国科学院成都分院 成都 640041)
  • 投稿日期:2007-03-26 修回日期:2007-05-15 发布日期:2007-08-28
  • 通讯作者: 钟国清

Synthesis, Crystal Structure and Thermal Decomposition of a Novel 3D Heterometallic Sb(III)-Pr(III) Complex [Sb2-μ4-(EDTA)2Pr(H2O)5]NO3•4H2O

SHEN Juan1; JIANG Qi-Ying1; ZHONG Guo-Qing*,1; JIA Yu-Qing2; YU Kai-Bei3   

  1. (1 Department of Chemistry, Southwest University of Science and Technology, Mianyang 621010)
    (2 Department of Chemistry, East China University of Science and Technology, Shanghai 200237)
    (3 Chengdu Branch of Chinese Academy of Sciences, Chengdu 640041)
  • Received:2007-03-26 Revised:2007-05-15 Published:2007-08-28
  • Contact: GuoQing Zhong

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合成了锑-镨与乙二胺四乙酸形成的新颖三维配合物[Sb2-μ4-(EDTA)2Pr(H2O)5]NO3•4H2O, 用元素分析、红外光谱、热分析及X射线单晶衍射法等进行了组成和结构表征. 结果表明该配合物属正交晶系, 空间群Pnn2; 晶胞参数: a＝1.07031(2) nm, b＝2.30805(4) nm, c＝0.72343(2) nm, V＝1.78711(7) nm3, Z＝2, Dc＝2.202 g/cm3, F(000)＝1164, μ＝2.955 mm－1, GOF＝1.000, 最终偏离因子R1＝0.0203, wR2＝0.0545 [I＞2σ(I)]. 在标题化合物中, 每个镨(III)离子的配位数为9, 与五个水分子中的五个氧原子和四个羧基氧原子配位, 形成三帽三角棱柱空间配位多面体. 锑(III)与EDTA离子中的四个氧原子和两个氮原子配位, 在赤道平面上有一孤对电子. 同时讨论了配合物的热分解过程.

关键词: 锑(III), 镨(III), 配合物, 晶体结构, 氨基羧酸

A novel 3D EDTA-linked (EDTA＝ethylenediamine-N,N,N',N'-tetraacetate) heterometallic antimony-praseodymium complex [Sb2-μ4-(EDTA)2Pr(H2O)5]NO3•4H2O has been synthesized and characterized by elemental analysis, FT-IR spectrum, TG-DSC and X-ray diffraction analyses. It crystallizes in the orthorhombic system, space group Pnn2 with a＝1.07031(2) nm, b＝2.30805(4) nm, c＝0.72343(2) nm, V＝1.78711(7) nm3, Z＝2, Dc＝2.202 g/cm3, F(000)＝1164, μ＝2.955 mm－1, GOF＝1.000, the final R1＝0.0203 and wR2＝0.0545 [I＞2σ(I)]. In the title complex, the Pr(III) ion is nine-coordinated. The coordination polyhedron around each praseodymium atom is a distorted tricapped trigonal prism with four oxygen atoms from four carboxylic groups and five oxygen atoms from five H2O molecules. The Sb(III) ion is coordinated by two N atoms and four O atoms from an EDTA, together with a lone electron pair in the equatorial position. It shows the possible pyrolysis reactions of experimental and calculated percentage mass losses in the thermal decomposition process.

Key words: antimony(III), praseodymium(III), complex, crystal structure, aminopolycarboxylic acid