Synthesis and Characterization of [Ir(<i>Acac^BiMs</i>)(COD)] and [<i>cis</i>-Ir(<i>Acac^BiMs</i>)₂(COE-OH)]

Abstract

The\nreaction of dinuclear complex [IrCl­(COD)]₂ (COD =\n1,5-cyclooctadiene) with 1 equiv of 1,3-dimesitylpropane-1,3-dione\n(H-<i>Acac</i>^<i>BiMs</i>) and an excess\nof triethylamine in benzene or dichloromethane at room temperature\nresults in the formation of β-diketonate complex [Ir­(<i>Acac</i>^<i>BiMs</i>)­(COD)], <b>1</b>. Further, compound <b>1</b> reacts with an equivalent\nof H-<i>Acac</i>^<i>BiMs</i> in dichloromethane\nunder atmospheric conditions to give the new complex with the formula\n[<i>cis</i>-Ir­(<i>Acac</i>^<i>BiMs</i>)₂(COE-OH)], <b>2</b> (COE-OH = σ,π-hydroxyenediyl),\nthrough a formal insertion of a hydroxyl group into a COD ring. All\ncompounds were characterized by melting point, analytical data, and\nIR and NMR spectroscopy. Additionally, an X-ray crystallographic study\nwas undertaken to corroborate the structure of both complexes.