Nicotinic and isonicotinic hydrazides and its derivatives have been the subject of interest to researchers of different profiles. Many of these ligands and their complexes have shown a wide spectrum of biological activity, including antibacterial and antiviral activities. Some of them have already been used in medical practice. Derivatives of isonicotinic acid and it hydrazides are well known for their highly specific antituberculous activity. In order to obtain complex compounds of this class, a new coordination compound, [NiL1L2], has been obtained as a result of the interaction of 2-hydroxi-1-naphtaldehyde nicotinoylhydrazone (L1) with 1-phenyl-1,3-butanedione isonicotinoylhydrazone (L2) in the presence of nickel acetate (in molar ratio 1:1:1) in methanol medium. The complex is less soluble in chloroform, dimethylformamide, dimethylsulfoxide, ethanol, methanol and water. Elemental analysis and the IR spectrosocopic data confirm the coordination of L1 and L2 molecules to nickel atom. The IR spectrum of the obtained ligands and coordination compound allowed making some conclusions about the composition, structure and status of the ligands in the complex. The spectrum of uncoordinated ligand L1 is characterized by a wide band with medium intensity at 3218 cm-1, which includes ν(NH) and ν(OH) associated oscillations and high intensity band at 1675 cm-1, assignable to ν(C=O) group. The band with medium intensity at 1624 cm-1 can be attributed to the ν(-CH=N-)azomet oscillations. For planar deformation oscillations of the 1,3-substituted benzene ring are assigned bands at 1082, 1162 and 1062 cm-1, and for joined three hydrogen atoms oscillations from the outside of the plane - a band at 780 cm-1. The C-H deformation oscillations of the hydrogen atom of aromatic ring from the outside of the plane were found a band at 843 cm-1, in the case of the isolated hydrogen atom. The most intensive absorption bands at 740 and 685 cm-1 in the spectra of L1 are assigned to deformation oscillations of C-H bonds of the aromatic rings. Phenol group of 2-hydroxy-1-naphthaldehyde can be identified by absorption bands ν(C-O) and δ(OH) situated in the spectrum at 1322 and 1274 cm-1. The IR spectrum of the second ligand L2 is characterized by the presence of two narrow and high intensity bands at 3220 cm-1 (ν(NH)) and 1664 cm-1 (ν( C=O)). For mono-substituted benzene ring are present bands at 738 and 714 cm-1 and for the pyridine ring, which is considered 1,4- disubstituted benzene ring - a band at 833 cm-1. The -CH3 group are identified by the bands at 2927 cm-1 (νas(CH3)) and 2837 cm-1 (νs(CH3)) and 1431 and 1379 cm-1 - δas and δs(CH3), respectively. The bands at 1595, 1574 and 1483 cm-1 are caused by the oscillations of the pyridine ring. In the IR spectrum of obtained complex [NiL1L2], with certainty, have not been identified absorption bands ν(NH) and ν(C=O), confirming the association and coordination of these group. This fact gives the allows us to conclude that ligands coordinate to the metal atom in the enolic form. Azomethine groups occur in the region 1617 cm-1. The presence of the pyridine ring is identified by the bands at 1602, 1584, 1480 and 772 cm-1. The monosubstituted benzene ring is confirmed by the presence of bands at 741, 730 and 681 cm-1. The most intensive absorption band of spectra at 1199 cm-1 could be caused by ν(CO) oscillations, incurred due enolization of coordinated ligands and participation of oxygen atoms and these groups to achievement of metal - ligand bonds.