摘要
本文根据分子碎片结合原理,用直接法由简单的单质元素,金属盐类及配体,通过控制反应温度,压力,时间及配体用量在CO气氛下一步合成含羰基和不含羰基的簇合物:Pd_3(SC_6H_4OH)_3(PPh_3)_3(OH)_2Cl(1),Fe_2S_2(CO)_5Pd(PPh_3)_3(2),Fe_2S_2(CO)-5Pt(PPh_3)_3(3).对它们进行了IR,NMR,EDS,元素分析,金属分析和化合物1的X光单晶衍射结构分析.化合物1属单斜晶系,离子型,P2_1/n空间群,晶胞参数a=1.4629(3)nm,b=1.9263(3)nm,c=2.4908(7)nm,β=94.53(2)°,Z=4,R=0.053.
According to the principle of fragment combination, the metal clusters of (SC6H4OH)3(PPh3)3(OH)2Cl(1),Fe2S2(CO)5Pd(PPh3)3(2), and Fe2S2(CO)5Pt(PPh3)3(3) which with carbonyl or without carbonyl groups are prepared under CO atmosphere by one step method using simple elements, metal salts and ligands as starting materials through controlling the reaction temperature, pressure, time and the amount of ligands.These clusters are analysed by elements of C/H and metal, and characterized with IR, 1H NMR, EDS. The single crystal of cluster (1) is also analysed by X - ray diffraction. The results showed that it belongs to monoclinic system, P21/n space group, the cell parameters are a =1.4629(3)nm, b = 1.9263(3)nm, c = 2.4908(7)nm, β = 94.53(2)°, V = 6.9974nm3, Z = 4,Dc=1.47g·cm-3, R= 0.053, Rw = 0.065.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
1996年第5期440-446,共7页
Acta Chimica Sinica
基金
中国科学院上海有机化学研究所所金属有机开放实验室资助项目
