Three new polypyridine iridium(III) complexes [Ir III Cl(L)-(tterpy)](PF 6 ) 2 {L = phen (1), dpphen (2), and dmbpy (3) (5) and terpy (6)} were also prepared. Abbreviations of the ligands used here are phen = 1,10-phenanthroline, dpphen = 4,7-diphenyl-1,10-phenanthroline, bpy = 2,2Ј-bipyridine, dmbpy = 4,4Ј-dimethyl-2,2Ј-bipyridine, tterpy = 4Ј-(4-tolyl)-2,2Ј:6Ј,2ЈЈ-terpyridine, and terpy = 2,2Ј:6Ј,2ЈЈ-terpyridine. The syntheses, which were accomplished in typical reaction times of fifteen minutes by using a microwave oven, were easier than a previous method. The complexes were characterized by electrospray mass spectrometry, UV/Vis spectroscopy, and cyclic voltammetry (CV). The X-ray structures of the two complexes 5 and 6 were also obtained. Cyclic voltammograms of all the [Ir III Cl(L)(tterpy)] 2+ complexes showed that the first reduction occurred at around -0.67 V, which is attributed to the re-