The ligand benzil bis(4-methyl-3-thiosemicarbazone)LH2 reacts with K2PtCl4, both in the presence or in the absence of LiOH center dot H2O, to yield simultaneously the cyclometallated mesocate [Pt-2(mu-L)(2)]1 and the coordination monomeric compound [PtL]2, which can be easily separated by their different solubility. By contrast, reaction of Li2PdCl4 without base leads exclusively to the formation of the coordination compound [PdL] 3, while the use of LiOH center dot H2O permits the selective synthesis of the cyclometallated mesocate [Pd-2(mu-L)(2)]4. All the complexes have been characterized by the usual techniques, including X-ray single crystal diffraction that show all the metals to be four-coordinate in a square-planar arrangement, but 2 and 3 with a N2S2 environment while in 1 and 4 it is CNS2. The cytotoxic activity has been evaluated against the human lung carcinoma cell line NCI-H460, but the results show that the complexes are not active in this cell line. (C) 2010 Elsevier B. V. All rights reserved.