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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。
Rhodium trichloride and acetylacetone were heated to reflux in N, N-dimethylformamide medium to synthesize acetylacetonate dicarbonyl rhodium ([Rh (CO) 2 (acac)] 2) in one step. The yield Was 93%. The quantitative reaction of [Rh (CO) 2 (acac)] 2 with triphenylphosphine (PPh3) with n-butane afforded acetylacetone · triphenylphosphine · rhodium (Rh PPh3) (CO)) in 99% yield. [Rh (ac) 2] and Rh (acac) (PPh3) (CO) single crystals were respectively grown by gas phase diffusion method and solvent evaporation method. The results of elemental analysis showed that the product was the target compound. Their structures were characterized by X-ray single crystal diffractometer, and the crystal structure parameters were obtained. The results showed that the two compounds are triclinic. The space group P-1, [Rh (CO) 2 (acac)] 2 Dimer compound, Rh (acac) (PPh3) (CO) is a mononuclear complex.