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化学学报
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化学学报 ›› 1990, Vol. 48 ›› Issue (2): 116-120. 上一篇    下一篇

研究论文

一水合二甲基磷酸镧的合成和晶体结构

刘承敏;吴国庆;汤中佳;韩玉真;潘作华;施倪承;廖立兵   

  1. 北京师范大学化学系;北京大学物理化学研究所;中国地质大学北京研究生院
  • 发布日期:1990-02-15

Synthesis and crystal structure of lanthanum dimethyl phosphate monohydrate

LIU CHENGMIN;WU GUOQING;TANG ZHONGJIA;HAN YUZHEN;PAN ZUOHUA;SHI NICHENG;LIAO LIBING   

  • Published:1990-02-15

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用改进的重结晶及晶体与母液分离的方法合成了标题化合物La[PO2(OCH3)2]3·H2O, 其单晶的结构分析用Patterson 法及差值Fourier 合成, 并经分块矩阵最小二乘法对非氢原子进行修正解出,R=0.054, 属三斜品系, 空间群PI, a=11.342(4), b=10.399(4),c=9.619(3)A, a=62.01(3), β=72.39(3), λ=66.60(3),V=909.9(6)A3, Z=2, Dw=1.94g·cm^-^3。该晶体中每个La原子有七个氧原子配位, 其中六个氧原子分别由六个二甲基磷酸根提供, 另一个氧原子由水分子提供; 这个配位多面体呈扭曲的单帽三棱柱体, 远程结构呈二维网状, 系因每两个La 原子共用一个二甲基磷酸根离子延伸连接而成。

关键词: 晶体结构测定, 镧化合物, 磷酸盐, 甲氧基, 水合物, 最小二乘法, 重结晶

After improving the method of recrystn. and separation of crystals from the mother liquor, La[PO2(OMe)2]3, H2O was synthesized and isolated as single crystals. The compound is triclinic, space group P1, with a 11.342(4), b 10.399(4), c 9.619(3) ? a 62.01(3), b 72.39(3), and g 66.60(3)? Z = 2 for dc = 1.94. The final R = 0.054. Each La is coordinated by 7 O atoms from 6 di-Me phosphate and 1 H2( mol., resp., forming a distorted monocapped trigonal prism. Each di-Me phosphate ligand is shared by 2 La atoms, building up a 2 dimensional network. Atomic coordinates are given.

Key words: CRYSTAL STRUCTURE DETERMINATION, LANTHANUM COMPOUNDS, PHOSPHATE, METHOXY GROUP, HYDRATE, LEAST SQUARE METHODS, RECRYSTALLIZATION

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