摘要
用光谱法研究了Co[(C_2H_5O)_2PS_2]_3与吡啶的取代还原反应,测定了反应的平衡常数K=0.66±0.05(mol·dm^(-3))^(-3)。用X射线单晶衍射方法测定了Co[(C_2H_5O)_2PS_2]_2·2Py的晶体结构。晶体空间群为P2_(1/c),晶胞参数a=8.117(7),b=17.813(4),c=9.901(3)A;β=104.19(5)°; Z=2;晶体密度计算值D_o=1.406g·cm^(-3)。差热分析印证了标题化合物含二分子吡啶。提出了可能的取代还原反应的机理。
The stability constant of the title complex was obtained by spectrophotometric
method with value K=0.66±0.05(mol·dm^(-3)). The rate of the title reaction is very
slow. Three crystals with different colours, namely violet, pink and colourless, were
separated. Difference in structure of the violet and pink crystals were indicated by spec-
trophotometry and TG-DT analysis. The colourless crystal is a dimer [(C_2H_5O)_2PS_2]_2.
Mechanism of reduetive reaction was suggested. The structure of the violet crystal was
determined by X-ray diffraction analysis. The crystal belongs to monoclinic system. a=
8. 117 (7), b=17. 813 (4), c=9. 901 (3) A,β=104. 19 (5)°, V=1387. 8A^3, D_c=1. 406g·cm^(-3),
Z=2,F(000)=610_θ, Space group P2_(1/c). The crystal structure was resolved by heavy
atomic method with final R=0.051.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
1989年第7期623-627,共5页
Acta Chimica Sinica