Synthesis, Spectroscopic Characterization and X-Ray Crystal Structure of the Chloride-Bridged Face-Sharing Bioctahedral Diiridium Complex [HP-t-Bu2Me][Ir2Cl7(P-t-Bu2Me)2], a Possible Precursor of the Complex [Ir(H)(Cl)2(P-t-Bu2Me)2

Abstract

The reaction of an ethanolic suspension of [NH4]2[IrCl6] and P-t-Bu2Me, in the presence of HCl for 15h gives [HP-t-Bu2Me][Ir2Cl7(P-t-Bu2Me)2], 1, in 13.5% yield. The dinuclear complex 1 was characterized by elemental analyses, IR, 1H, 31P NMR spectroscopy, and single crystal X-ray analysis. However, when the above reaction is continued for 48 h one obtains only [Ir(H)(Cl)2(P-t-Bu2Me)2], 2, in good yield. It is proposed that complex 1 is a reaction intermediate to 2. Crystallographic data for 1 (at 298 K): a = 16.151(3) Å, b = 11.885(2)Å, c = 21.665(4) Å, β = 90.26(2)°, space group P21/c (Z=4).