【摘要】 在N,N-二甲基甲酰胺介质中,将水合三氯化铑与乙酰丙酮加热回流,一步合成了乙酰丙酮·二羰基铑([Rh(CO)2(acac)]2),产率为93%;以正丁烷为介质,[Rh(CO)2(acac)]2与三苯基磷(PPh3)定量反应,得到乙酰丙酮·三苯基膦·羰基铑(Rh(acac)(PPh3)(CO)),产率为99%。用气相扩散法和溶剂缓慢挥发法分别培养出[Rh(CO)2(acac)]2和Rh(acac)(PPh3)(CO)单晶,元素分析的结果表明产物为目标化合物。用X射线单晶衍射仪对其结构进行了表征,获得了晶体结构参数,结果表明2种化合物均为三斜晶系、P-1空间群,[Rh(CO)2(acac)]2为二聚体化合物,Rh(acac)(PPh3)(CO)为单核配合物。更多还原

【Abstract】 [Rh(CO)2(acac)]2 was synthesized in one-step process from Rh Cl3·3H2O in DMF by adding acac as the anion ligand. The yield was 93%. A quantitative reaction between [Rh(CO)2(acac)]2 and PPh3 in n-butane gave rise to the formation of Rh(acac)(PPh3)(CO) with a yield of 99%. Single crystals of two complexes were prepared, respectively, via a gaseous diffusion method and a solvent evaporation technique, and were subjected to X-ray diffraction analysis. The results show both complexes are in the triclinic system with a space group of P-1. [Rh(CO)2(acac)]2 displays a dimmeric structure with Rh-Rh bond being 3.417 ?, whereas Rh(acac)(PPh3)(CO) has a normal mononuclear structure.更多还原