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本文通过Co_2(CO)_8与5个取代硫脲R~1NHC(S)NHR~2反应,制得了通式为Co_3(CO)_7(μ3-S)[μ-η~2-R~1NC(S)NHR~2]5个新簇合物.除用碳氢氮元素分析、IR、~1H NMR和MS表征它们的结构外,还用X光衍射法测得R~1=Ph,R~2=CH_2Ph簇合物的单晶结构.该簇合物属三斜晶系,PI空间群.晶胞参数如下:a=0.9116(1),b=1.2289(2),c=1.2518(2)nm,α=115.56(1),β=100.94(2),γ=93.39(1)°;Z=2;V=1226.2×10~(-3)nm~3;D_c=1.750g·cm~(-3);μ=22.099cm~(-1);F(000)=646.结构分析表明,该分子中的Co_3S原子构成三角锥分子骨架,所有CO为钴原子的端羰配体,而PhNC(8)NHCH_2Ph以S原子和与苯基相连的N原子分别与两个钴原子配位,形成Co_2NCS五圆环结构.
In this paper, the reaction of Co_2 (CO) _8 with 5 substituted thioureas R ~ 1NHC (S) NHR ~ S) NHR ~ 2] were synthesized and characterized by X-ray diffractometry in addition to the analysis of their structures by means of the analysis of hydrocarbon nitrogen, IR, ~ 1H NMR and MS. 2 = CH_2Ph cluster. The cluster is a triclinic system in the space group of PI with unit cell parameters of a = 0.9116 (1), b = 1.2289 (2), c = 1.2518 (2) nm, α = 115.56 (1), β = 100.94 (2), γ = 93.39 (1) °, Z = 2, V = 1226.2 × 10 -3 nm 3, D c = 1.750 g · cm -1 -3); μ = 22.099cm -1; F (000) = 646. The structural analysis shows that the Co_3S atom in the molecule constitutes the triangular pyramid molecular skeleton, and all the COs are terminal carbonyl ligands of the cobalt atom. PhNC (8) NHCH_2Ph coordinated with two cobalt atoms by S atom and N atom connected with phenyl respectively to form Co_2NCS five-ring structure.