The synthesis of nickel and zinc complexes of the ligand 2,4-diiodo-6-(((2-pyridinylmethyl)amino)methyl)phenol is reported. Various spectroscopic, spectrometric, and structural methods are used in their characterization, and their pharmacological effects were evaluated in vitro and in cultured human cancer cells in terms of proteasome-inhibitory and apoptosisinducing capabilities.