For some time, isonicotinic hydrazide and its derivatives has been a subject of interest to researchers of different profiles. Many of these ligands and their complexes have shown a wide spectrum of biological activity, such as antibacterial, antiviral activities, several of them are already used in medical practice. Two new organic ligands resulting from isonicotinic hydrazide and acetylacetone (1) or benzoylacetone (2) have been prepared and investigated by different modern physico-chemical methods (including elemental analysis, 1H and 13C NMR, IR and X-ray investigations) (fig. 1 and 2). figure Fig. 1. Structure of molecule 1 Fig. 2. Structure of molecule 2These base Schiff are soluble in chloroform, DMF, DMS, EtOH, MeOH, low soluble in water (melting point 131-133°C and 145-147 °C, respectively for 1 and 2). The absence of the bands at 3150-3400 cm-1 in the IR spectra of the compounds indicates that the NH2 group reacts with the aldehyde. The C=C and C=N stretching vibrations are exhibited at 1622.6 and 1506.9 cm–1, respectively for compound 1 and 2. The 1H NMR and 13C NMR spectra of solutions in CDCl3 showed the presence of all atoms of hydrogen and carbon predicted by the molecular formula 1 and 2. The X-ray investigation revealed that the condensation of acetylacetone with isonicotinic hydrazide is accompanied by a cycle formation consist of five atoms: three carbon atoms of acetylacetone and two nitrogen atoms of isonicotinic hydrazide fragment, with the following atoms distances: C(2)-N(1) = 1.278(3), N(1)-N(2) = 1.398(3), C(4)–N(2) = 1.507(3), C(4)–C(3) = 1.533(4) and C(3)–C(2)(4) = 1.476(4) (Å). The cyclization was not observed in molecule 2, condensation between benzoylacetone and isonicotinic hydrazide occurs in 1:1 ratio with the formation of Schiff ligang 2. The atoms distance C(9A)N(1A) = 1.368(5), N(1A)-N(2A) = 1.402(6), C(7A)-O(01A) = 1.268(5) and N(2A)-C(11A) =1.348(5) (Å).