Binuclear complexes of Rh and Ir containing a flexibly bridging bis (2, 4-pentanedionato) ligand have been synthesized and characterized. The reaction of [M (r-Cl)(1, 5-COD)] 2 (M= Rh, Ir) with p-xylylenebis (3-(2, 4-pentanedione)),~ yl (Hacac)~, and 2 equiv of KOH results in the formation of the binuclear compounds (M (COD)),(xyl (acac),). The cyclooctadiene ligand in these complexes is readily displaced from the metal centers by either CO or PPh, ...