环己基甲酸镧配合物的合成与晶体结构的研究

A STUDY ON THE SYNTHESIS AND CRYSTAL STRUCTURE OF LANTHANUM (Ⅲ) COMPLEX WITH CYCLOHEXANE CARBOXYLIC ACID

本文合成了环己基甲酸镧配合物Ｌａ（Ｃ６Ｈ１１ＣＯＯ）３·（Ｃ６Ｈ１１ＣＯＯＨ）·１．５Ｈ２Ｏ，晶体属三斜晶系，Ｐ１空间群，晶胞参数：ａ＝１５．３３１（４），ｂ＝１５．５５５（４），ｃ＝１６．８３３（５）；α＝１０５．４８（２）°，β＝９６．４８（２）°，γ＝１１０．２１（２）°，Ｖ＝３５３６．９（１４）３；Ｚ＝４，Ｄｃ＝１．２６９ｇ／ｃｍ３。经全矩阵最小二乘法修正，最终偏差因子Ｒ为０．０６２７。晶体中镧原子之间分别由两个和三个羧基桥连，形成链状聚合分子，镧原子的配位数为１０，配合物为变形的双帽四方反棱柱构型。

? A study on the synthesis, crystal and molecular structure of La(C 6H 11 COO) 3·(C 6H 11 COOH)·1.5 H 2O is presented in this paper. The crystal and molecular structure and determined by the singlecrystal Xray diffraction method with a four circle diffractometer to give a final R value of 00627 [I>2σ(I)]. The crystal is in triclinic with space group P1. The unit cell parameters are as follows: a=15.331(4),b=15.555(4), c=16.833(5);α=105.48(2)°, β=96.48(2)°, γ=110.2(2)°, V=3536.9(14) 3; Z=4. Each lanthanum atom with its two neighboring lanthanum atoms are connected with two and three tridentatetype bridging carboxyl groups respectively, to form a chain polymeric molecule. There are two types of independent lanthanum atoms, with same coordination number (N=10), and their coordination polyhedrons all take an arrangement of a distorted bicapped square antiprism. In the complex, the coordinating oxygen atoms are classified into three types, that is, chelating carboxyl group, tridentate bridging carboxyl group and coordinating water molecule. In the crystal, free acid molecules are hydrogenbonded to the oxygen atoms of the coordinated water molecule and the coordinated carboxyl group through its carboxyl oxygen atoms.