A rhodium(iii) complex, [Rh(MQ)(DMSO)Cl] (), with 8-hydroxy-2-methylquinoline as the ligand was synthesized and characterized. Complex exhibited cytotoxicity against BEL-7404, Hep-G2, NCI-H460, T-24, and A549 cell lines with IC values in the micromolar range (6.52-17.86 μM). Various experiments on the Hep-G2 cells showed that complex caused cell cycle arrest at the S phase, downregulation of cdc25 A, cyclin A, cyclin B and CDK2, and upregulation of p21, p27 and p53. Furthermore, cytotoxicity mechanism studies suggested that complex-induced apoptosis was achieved disruption of the mitochondrial function, which led to a significant loss of the mitochondrial membrane potential, an increase in the cellular levels of reactive oxygen species, cytochrome c, and apaf-1, and a fluctuation of the intracellular Ca concentration. Taken altogether, complex can trigger cancer cell death by inducing apoptosis through a mitochondrial dysfunction pathway.