New and improved procedures are reported for the synthesis of [M(DBCOT)(μ-Cl)] 2 (M=Rh, Ir; DBCOT=dibenzo[a,e]cyclooctatetraene) from MCl 3 (H 2 O) x or [M(COD)(μ-Cl)] 2 and DBCOT. Treatment of [M(DBCOT)(μ-Cl)] 2 with [(LAu) 3 (μ-O)]BF 4 (L=PPh 3 , P t Bu 3 ) yields the mixed-metal oxo complexes [M(DBCOT)(μ 4 -O)(AuL) 2 ] 2 (BF 4 ) 2 . Dimeric [Rh(DBCOT)(μ-OH)] 2 is obtained from the reaction of [M(DBCOT)(μ-Cl)] 2 with KOH in EtOH/H 2 O. All complexes except [Rh(DBCOT)(μ-Cl)] 2 have been structurally characterized by single crystal X-ray diffraction.