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Half-sandwich organorhodium(III) complexes and their trichloridorhodium(III) counterparts are potent anticancer agents that enhance the formation of reactive oxygen species and invoke a strong induction of apoptosis in leukemia cells. The antiproliferative activity towards human MCF-7 and HT-29 adenocarcinoma cells of novel nonintercalating complexes containing the 5-substituted phenanthroline ligands 5,6-dimethylphenanthroline, 5-chlorophenanthroline, and 5-nitrophenanthroline (phen*) increases dramatically in the order [(η⁵-C₅Me₅)IrCl(phen*)](CF₃SO₃) < [(η⁵-C₅Me₅)RhCl(phen*)](CF₃SO₃) < mer-[RhCl₃(DMSO)(phen*)] (DMSO is dimethyl sulfoxide) . Improved activity was also achieved by attaching a cell-penetrating peptide to the dipyrido[3,2-a:2′,3′-c]phenazine (dppz) ligand of an organorhodium(III) complex. Whereas 5-substitution led to significant improvements in the activity of the …