The aim of this work is the synthesis, determination of the composition, structure, physicochemical, antimicrobial and antifungal properties of 2-hydroxy-3methoxybenzaldehyde 4-(2,4-dimethylphenyl)thiosemicarbazone (H2L1) and 4-(3,4dimethylphenyl)thiosemicarbazone (H2L2) as well as iron(III), cobalt(III), nickel(II), and copper(II) coordination compounds with these ligands. The thiosemicarbazones H2L1-2 react with chlorides, bromides, nitrates and perchlorates of stated above metals forming colored solutions. Upon cooling the precipitates of coordination compounds are formed: Cu(HL1-2)X • nH2O (X = Cl-, Br-, ClO4-, NO3-, n = 0, 4), Co(HL1-2)2X (X = Cl-, NO3-), Cu(L1-2)H2O, Fe(HL1)2X • nH2O (X = Cl-, NO3-; n = 0, 2), Ni(L1-2)H2O. The composition and structure of these compounds were determined using elemental analysis, magnetochemical research and IR-spectroscopy. It was determined that all coordination compounds have monomeric structure. The thiosemicarbazones H2L1-2 act as tridentate ligands with O, N, S set of donor atoms. Synthesized coordination compounds show selective antimicrobial activity towards a series of standard strains of Staphylococcus aureus, Escherihia coli, and Candida albicans in the range of concentration 0.0039-0.5 mg/mL. It was shown that the nature of the central atom has a main influence on the antimicrobial activity of these complexes. For the homotypic complexes the activity diminishes in the following way: Cu > Ni > Co ≥ Fe. The nature of thiosemicarbazone and acid residue also has an influence on antimicrobial activity. The antimicrobial activity reduces in the following way: H2L1 > H2L2 and NO3- > ClO4-> Cl- ≥ Br-. Synthesized compounds manifest the best activity towards the standard strains of Staphylococcus aureus and Candida albicans.