The synthesis and characterization of new bis-cyclometalated complex salts [Ir(ptpy)(2)(L-phen)]PF6 with L-phen = 2,9-dimethyl-4,7-bis(pentyloxy)-1,10-phenanthroline (1) and L-phen = 2,9-dimethyl-4,7-bis(2-ethoxyethoxyl)-1,10-phenanthroline (2) are described. Compounds 1 and 2 were obtained by the reaction of the corresponding phenanthroline ligands with [{Ir(mu-Cl)(ptpy)(2)}(2)] in a refluxing CH2Cl2/MeOH mixture. The molecular structure of compound 2 was confirmed by single-crystal X-ray structure determination. Complex 2 was crystallized from dichloromethane/methanol/iso-hexane in the monoclinic space group P2(1)/c. The biological activity of both new compounds was examined, and they exhibit significant cytotoxicity against human cancer cell lines with the IC50 values around 2 mu M, significantly better than the established anticancer drug cisplatin under identical conditions.