Chemistry of the metal carbonyls. Part LIV. Synthesis of rhodium and iridium carbonyls

Abstract

Dodecacarbonyltetrarhodium has been prepared (60–70% yield) by treating [Rh(CO)₂Cl]₂ in hexane with carbon monoxide at 200 atmos. at room temperature in the presence of copper wire. The hexanuclear carbonyl Rh₆(CO)₁₆ has been synthesized in 80–90% yield by reacting methanolic solutions of rhodium trichloride trihydrate with carbon monoxide at 40 atmos. and 60°. By varying the concentrations [Rh(CO)₂Cl]₂ is obtained in 80% yield. Dodecacarbonyltetrairidium has been prepared in ca. 60% yield by carbonylating a methanolic solution of iridium trichloride with carbon monoxide at 40 atmos. (60°). The mass spectrum of Rh₆(CO)₁₆ has been measured.