Two new tetracationic hetero-bimetallacycles, 4 and 5, have been constructed from an N,N′-bis(4-(pyridin-4-ylethynyl)phenyl)pyridine-2,6-dicarboxamide ligand, 1, and cis-blocked complexes [M(dppf)](OTf)2 (dppf = 1,1′-bis(diphenylphosphino)ferrocene; M = Pd (2), Pt (3)) in CH3NO2/CH2Cl2 (1:1) solvent. Both complexes were isolated with adequate yields as triflate salts and were then characterized using 1H, 13C, and 31P NMR spectroscopy, elemental analysis, UV-Vis spectroscopy, and high-resolution electrospray mass spectrometry (HR-ESMS). The molecular structure of 4 was determined by molecular mechanics force field calculations. The cytotoxic effect of both new complexes were analyzed against T98G (brain tumor), KB (head and neck cancer), SNU-80 (thyroid cancer), and HEK-293 non-malignant cell lines. The cytotoxicity of complexes 4 and 5 were found to be considerably more effective against cancer cells than reference drug cisplatin. Annexin-V/PI staining, caspase-3/-7 activity, reduction in mitochondrial membrane potential justify a significant level of apoptosis in complex treated cells.