The structures of iron(III) and nickel(II) complexes with the composition [FeL 2 ]Cl⋅H 2 O (1) and[Ni( 2 HL ′ )]⋅DMSO⋅0.5H 2 O (2), where L and HL′ are monodeprotonated residues of 1′-phthalazinylhydrazones of 2-acetyl benzimidazole and 1-phenyl-3-methyl-4-formyl-5-hydroxypyrazole respectively, are determined using single crystal X-ray diffraction analysis. Both compounds crystallize in the monoclinic symmetry. The Fe(III) and Ni(II) ions in the complexes have octahedral N 6 and N 4 O 2 donor environments respectively. Due to intermolecular hydrogen bonds, the molecules of the complexes form corrugated (complex 1) and linear (complex 2) molecular chains in the crystal.Intensive study of transition metal complexes with hydrazones based on 1-hydrazonophthalazine (hydralazine) is primarily due to the biological activity displayed by hydrazones themselves and their complexes [1][2][3][4][5][6]. The possibility of a bidentate or tridentate coordination of 1′-phthalazinylhydrazones in different tautomeric forms predetermines a wide variety of the forms of the complexes whose composition depends on the structural features of the ligand, synthesis conditions, and the nature of the complexing metal [6][7][8][9][10]. Unlike the majority of other hetarylhydrazones, 1′-phthalazinylhydrazones can also act as chelate-bridging N,N′ donor ligands, which enables the preparation of binuclear complexes based on them [11,12].This work is a continuation of the study of the complexing ability of phthalazinylhydrazones of polyfunctional carbonyl compounds [10][11][12][13][14]. Here we report the results of the single crystal X-ray diffraction analysis of iron(III) and nickel(II) complexes with 1′-phthalazinylhydrazones of 2-acetyl benzimidazole (HL) and 1-phenyl-3-methyl-4-formyl-5hydroxypyrazole (H 2 L′).