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Treatment of THF solutions containing the rhodium(II) complex  trans -[RhCl 2 (P  t  Bu 2 Ph) 2 ] ( 1 ) with [Fe 2 (CO) 9 ] in the same solvent resulted in the formation of the Vaska-type complex  trans -[RhCl(CO)(P  t  Bu 2 Ph) 2 ] ( 2 ) in high yield. The title complex  2  was obtained as pale yellow crystals, characterized by NMR and IR spectroscopy, as well as by microanalyses. Additionally, the molecular structure of  2  has been established by X-ray crystallography. As often reported for similar constituted compounds, the chlorido and carbonyl ligands in crystals of  2  are strongly disordered.

Crystal and molecular structure of trans -[RhCl(CO)(P t Bu 2 Ph) 2 ]