高等学校化学学报

高等学校化学学报 ›› 1988, Vol. 9 ›› Issue (5): 432.

• 论文 • 上一篇    下一篇

Co[(C2H5O)2PS2]3·1/2H2O的合成和分子结构

徐正1, 俞运鹏1, 林建华1, 徐洁1, 游效曾1, 林墀昌2, 刘世雄2   

  1. 1. 南京大学配位化学研究所;
    2. 福州大学结构化学研究室
  • 收稿日期:1986-04-09 出版日期:1988-05-24 发布日期:1988-05-24
  • 通讯作者: 徐正

Synthesis and Crystal Structure of Tri-(O,O' -Diethyldithiophosphato) Cobalt(Ⅲ)

Xu Zheng1, Yu Yunpeng1, Lin Jianhua1, Xu lie1, You Xiaozeng1, Lin Chichang2, Liu Shixiong2   

  1. 1. Coordination Chemistry Institute, Nanjing University, Nanjing;
    2. Institute of Structural Chemistry, Fuzhou University, Fuzhou
  • Received:1986-04-09 Online:1988-05-24 Published:1988-05-24

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摘要： 用光谱法研究了双-(O,O'-二硫代磷酸酯)合钴(Ⅱ)的氧化过程。用电子光谱、光电子能谱、差热-热重分析和质谱等对氧化产物进行了表征。并用X射线衍射法测定了晶体结构。晶体属三斜晶系,空间群为P1,晶胞参数为:α=9.805(1)Å,b=9.812(2)Å,c=14.271(2)Å,α=89.46(2)°,β=89.42(1)°,γ=86.95(2)°,V=1370.9Å3,Z=2,Dc=1.509g·cm-3,F(000)=645e。Co(Ⅲ)与三个二硫代磷酸酯形成六配位的八面体配合物。

关键词: 二乙基二硫代磷酸酯, 钴配合物, 晶体结构, 分子结构, X射线衍射分析

Abstract: Oxidation process of CoC(C2H5O)2PS2]2 was studied by UV-Vis method to get the title compound. The rate of oxidation reaction is very slow and seems depending on alkyl group in the ligand molecule. The oxidation product CoC(C2H5O)2PS2]3·1/2 H2Owas characterized by UV-Vis, MS, TG-DTand PES.The crystal of CoC(C2H5O)2PS2]3 · 1/2 H2O belongs to Iriclinic, space group P1, parameters of unit cell are:α= 8.805(1)Å, b=9.812(2)Å, c = 14.271(2)Å, α = 89.46(2)°, β=89.42(1)°, γ=86.95(2)°, F=1370.9Å3, Z=2, Dc = 1.509g·cm-3, F(000) = 645e, final R= 0.080 for 4279 reflections with I≥3σ(Ⅰ) bond lengths of Co-Sare 2.319 + 0.004Å. Bond angles of cobalt atom and two sulphur atoms in the same dithiophosphate group are 85.07~85.35°. Bond angles of cobalt atom and any two neighbour sulphur atoms which are not in same dithiophosphate group are 89.35 - 95.35 °.There have three oxygen atoms of crystal water with 1/6 possibility for each in unsymmetry unit. Nonbonding distances between these oxygen and sulphur atoms are 2.12~2,27Å, which are much less than the sum of the van der Waals radii. It shows that some kinds of hydrogen bonds such as O—H...S are present.

Key words: Diethyldithiophoshate, Co complex, Crystal structure, Molecular structure, X-ray diffraction analysis

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