Synthesis and characterisation of [N(PPh3)2][RuRh5(CO)16] by X-ray crystallography and by natural-abundance carbon-13 nuclear magnetic resonance spectroscopy

Abstract

The synthesis, X-ray crystal structure, and spectroscopic studies of a new ruthenium–rhodium mixed-metal cluster [N (PPh₃)₂][RuRh₅(CO)₁₆] are reported. The complex crystallises in the space group C2/c with a= 33.62(1), b= 9.729(2), c= 33.72(1)Å, β= 94.43(2)°, and Z= 8. The crystal structure is isomorphous with [N(PPh₃)₂][FeRh₅(CO)₁₆]. No fluxionality was observed at room temperature by natural-abundance ¹³C n.m.r. spectroscopy, which established the [Rh₆(CO)₁₆]-like structure also in solution.