希土羧酸盐的结构研究——Ⅲ.[Y(n-C5H11COO)3·2H2O]2的合成和结构测定
STRUCTURAL STUDIES ON RARE EARTH CARBOXYLATES ⅡI. THE SYNTHESIS AND STRUCTURE DETERMINATION OF [Y(n-C5H11COO)3·2H2O]2
作者单位
张德龙 北京大学化学系希土化学研究中心, 北京 100871 
黄春辉 北京大学化学系希土化学研究中心, 北京 100871 
徐光宪 北京大学化学系希土化学研究中心, 北京 100871 
郑启泰 中国医学科学院药物研究所, 北京 100050 
贺存恒 中国医学科学院药物研究所, 北京 100050 
摘要: 本文合成了系列配合物Ln(n-C5H11COO)3·2H2O(Ln=Y,Sm,Eu,Gd,Tb,Er和Yb),并对[Y(n-C5H11COO)3·2H2O]2的晶体结构进行了研究。结果表明该晶体属于单斜晶系,P21/α空间群。晶胞参数如下:a=8.925(6),b=14.033(5),c=19.988(6)Å;β=95.90(3)°;V=2490.3Å3,Z=2.2978个独立可观察点(Ⅰ>3σ(Ⅰ))参加了结构修正,最终R因子为0.085。分子中1两个Y原子通过两个μ2-C5H11COO桥基连结成双核配合物;每个Y还与两个双齿螯合的羧基和两个水分子成键。因此Y原子的配位数为9。对系列化合物的红外光谱也进行了研究。
关键词: 正已酸    合成  晶体结构
基金项目: 中国自然科学基金
Abstract: A scries of complexes Ln(n-C5H11COO)3·2H2O, where Ln = Y, Sm, Eu, Gd, Tb, Er and Yb, have been synthesized. Their similarities in composition and structure have been confirmed by the elemental analysis and FT-IR spectra. As a representative of these complexes, the crystal and molecular structure of titled complex has been determined by single crystal X-ray diffraction techniques with a four circle diffractometer. 2978 independent reflections [I>3σ(I)] were used for the structure refinement to give a final R value of 0.085. The crystal is in monoclinic with a space group P21/a. The unit cell parameters are: a= 8.925(6), b= 14.033(5), c= 19.988(6)Å; β = 95.90(3)°; V=2490.3Å3; Z= 2.In the molecule, two Y atoms are connected by two u2-bridging carboxylic groups to form a dimer. The non-bonding distance between Y-Y is 4.086(2)A. The middle point of Y-Y linking line is the symmetrical center of the molecule. Each Y atom is coordinated by nine oxygen atoms, of which, two from two water molecules; four from two chelate carboxylic groups and the rest three are provided by a u2-bridging carboxylic group. The average bond length for Y-O(H2O) and Y-O (chelate carboxylic groups) are 2.350 and 2.431Å respectively; and the bond lengths related with u2-bridging carboxylic group is 2.460, 2.366 and 2.504Å.
Keywords: n-pentanoic acid  Y  synthesis  crystal structure
投稿时间:1989-09-01 
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张德龙,黄春辉,徐光宪,郑启泰,贺存恒.希土羧酸盐的结构研究——Ⅲ.[Y(n-C5H11COO)3·2H2O]2的合成和结构测定[J].无机化学学报,1992,8(1):22-27.
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