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The S-methyl-thiosemicarbazones of the 2-hydroxy-R-benzaldehyde (R= H, 3-OH 3-OCH₃ or 4-OCH₃) reacted with the corresponding aldehydes in the presence of FeCl₃ and NiCl₂. New ONNO chelates of iron(III) and nickel(II) with hydroxy- or methoxy-substitued N ¹,N ⁴-diarylidene-S-methyl-thiosemicarbazones were characterized by means of elemental analysis, conductivity and magnetic measurements, UV-Vis, IR and ¹H-NMR spectroscopies. Cytotoxic activities of the compounds were determined using K562 chronic myeloid leukemia and ECV304 human endothelial cell lines by MTT assay. It was determined that monochloro N ¹-4-methoxysalicylidene-N ⁴-4-methoxysalicylidene-S-methyl-thiosemicarbazidato-iron(III) complex showed selective anti-leukemic effects in K562 cells while has no effect in ECV304 cells in the 0.53 μg/ml (IC₅₀ …