Ir(nbd2)(bipy)(acac) (F.W. = 632 for IrC29H31N2O2). Anal. Calc. for [Ir(nbd2)(bipy)(acac)] × 1.5 CH2Cl2 (F.W. = 724): C 48.2%, H 4.5, N 3.7. Found: C 47.9, H 5.6, N 3.6. ESI-MS shows that under these conditions ligand exchange and ligand loss can occur. Most prominent are the molecule Ir(nbd2)(bipy)2(acac) and the cation [Ir(nbd2)(bipy)2]+: Ir(nbd)2(bipy)2(acac) + H+ (789 with 193Ir and 787 with 191Ir); [Ir(nbd2)(bipy)2]+ (689 with 193Ir and 687 with 191Ir).