from 120.4(5) to 121.8(5)°. The coordination polyhedrons of the Pd atoms are close to square planar ones. The reaction of the Pd4(CO)4(OCOCF3)4 clusters with nitrogen monoxide leads to a substitution of the carbonyl groups and formation of the low stable complex Pd4(NO)4(OCOCF3)4 (III) that was characterized by the spectroscopic and analytical data. The transformation of III during slow recrystallization
摘要合成了两种亚硝基
羧酸钯钯配合物,并通过X射线衍射分析等方法对其结构进行了表征。通过Pd(NO)Cl与
羧酸银Ag(OCOR)反应合成了四核配合物Pd4(μ-NO)2(OCOR)6(分别为R = CMe3,Me,Ph,CHMe2,
CH2Cl,IIa–e) )。通过单晶X射线衍射法确定IIa的结构。IIa的晶体是单斜晶,空间群P21 / n,a = 12.104(7),b = 23.970(8),c = 15.495(4)A,β= 90.30(4)°,V = 4496(4)A3。对于6228次反射,在F2上的最小二乘结构细化收敛到R = 0.0714 [I>2σ(I)]。在IIa中,
钯原子在规则矩形Pd4附近形成,其边缘由
配体桥接。占据矩形相对侧的两个桥接NO基团相对于Pd4平面处于顺式位置。这些基团是对称的,PdNO角范围为120.4(5)至121.8(5)°。Pd原子的配位多面体接近