Thiosemicarbazones compose an important class of ligands with N, S-donor atoms because of their highly interesting chemical, biological and medicinal properties.1 Metals can bond to this kind of ligands and form chelate rings that are similar to structures that occur between metal ions and many important biological molecules such as proteins, enzymes and DNA.2 In this work 10 new coordination compounds of 1-(piperidin-1-yl)propane-1,2-dione 4allylthiosemicarbazone (HL) with such metals, like copper(II), cobalt(III), iron(III), nickel(II), and zinc(II) are presented. The purity and structure of the synthesized thiosemicarbazone was determined using NMR spectroscopy and X-ray diffraction analysis. Coordination compounds were synthesized by reaction between ethanol solutions of this thiosemicarbazone and metal salts in a molar ratio of 1:1 for copper and 2:1 for cobalt, nickel, iron, and zinc. Also three amine-containing coordination compounds were synthesized The composition of the synthesized complexes was established based on metal analysis data: Cu(L)X (X=Cl-, Br-, NO3 -); Fe(L)2Cl; Co(L)2Br; Ni(HL)2(NO3)2; Zn(L)2; Cu(1,10Phen)(HL)(NO3)2; Cu(1,10-Phen)(L)NO3; Cu(2,2’-BPy)(L)NO3. The study of molar electrical conductivity showed that the complexes of nickel and Cu(1,10-Phen)(HL)(NO3)2 are electrolytes of the 1:2 type, the complex Zn(L)2 is a nonelectrolyte, and all other complexes are electrolytes of the 1:1 type. According to the IR spectra of the synthesized compounds, it was found that thiosemicarbazone HL in complexes behaves as a tridentate ligand with ONS-set of donor atoms, forming two metallacycles of six and five atoms.