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

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, D_c＝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.

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

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, D_c＝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.