摘要
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[PO_2(OCH_3)_2]_3·H_2O,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。属三斜晶系,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),γ=66.60(3)°,v=909.9(6)A^3,z=2,D_x=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。
After improving the method of recrystallization and separation of crystals from the mother liquor, the title complex La[PO_2 (OCH_3)_2]_3·H_2O has been synthesized and isolated as single crystals. The crystal structure belongs to triclinic, space group P1 with a=11.342(4), b=10.399(4), c=9.619(3)(?), α=62.01(3), β=72.39(3), γ= 66.60 (3)~0,Ⅴ=909.9(6)(?)~3,Z=2,D_(?)=1.94g·cm^(-3). The structure was solved by Patterson method and refined by block least squares routine for nonhydrogen atoms. The final deviation factor R is 0.054. The analysis shows that each lanthanum atom is coordinated by seven oxygen atoms from six dimethyl phosphate and one water molecule respectively, forming a distorted monocapped trigonal prism. Each dimethyl phosphate ligand is shared by two lanthanum atoms, building up a two dimensional network.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
1990年第2期116-120,共5页
Acta Chimica Sinica
