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

Abstract

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, D_c = 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

TrendMD:

Xu Zheng, Yu Yunpeng, Lin Jianhua, Xu lie, You Xiaozeng, Lin Chichang, Liu Shixiong. Synthesis and Crystal Structure of Tri-(O,O' -Diethyldithiophosphato) Cobalt(Ⅲ)[J]. Chem. J. Chinese Universities, 1988, 9(5): 432.

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