Synthesis and Characterization of [Ir(AcacBiMs)(COD)] and [cis-Ir(AcacBiMs)2(COE-OH)]

The reaction of dinuclear complex [IrCl­(COD)]2 (COD = 1,5-cyclooctadiene) with 1 equiv of 1,3-dimesitylpropane-1,3-dione (H-AcacBiMs) and an excess of triethylamine in benzene or dichloromethane at room temperature results in the formation of β-diketonate complex [Ir­(AcacBiMs)­(COD)], 1. Further, compound 1 reacts with an equivalent of H-AcacBiMs in dichloromethane under atmospheric conditions to give the new complex with the formula [cis-Ir­(AcacBiMs)2(COE-OH)], 2 (COE-OH = σ,π-hydroxyenediyl), through a formal insertion of a hydroxyl group into a COD ring. All compounds were characterized by melting point, analytical data, and IR and NMR spectroscopy. Additionally, an X-ray crystallographic study was undertaken to corroborate the structure of both complexes.