Three new coordination complexes, 2{[Co (L 1 ) 2 ]ClO 4 } Á 0.5CH 3 OH (1), [Mn(L 2 ) 2 ] (2), and [Cu(HL 2 ) (L 2 )]ClO 4 Á 2H 2 O (3) have been synthesized from two tridentate N,N,O-donor hydrazone ligands HL 1 , 2-acetylpyridine-salicyloylhydrazone, and HL 2 , 2-benzoylpyridine-salicyloylhydrazone, respectively and thoroughly characterized by elemental analysis, FT-IR, UV-Vis, electrochemical, and room temperature magnetic susceptibility measurements. Structures of the complexes have been unequivocally established by single crystal X-ray diffraction technique. Structural analysis reveals that 1 consists of two chemically similar but crystallographically independent cationic [Co(L 1 ) 2 ] ? units and 2 consists of a neutral [Mn(L 2 ) 2 ] molecule while 3 consists of a cationic [Cu(HL 2 )(L 2 )] ? unit. Metal ions display distorted octahedral geometry in 1 and 2 while in 3 it shows a distorted square pyramidal geometry. Ligand conformations around the metal ions are stabilized by the presence of intra-ligand hydrogen bonding in all the complexes. Structure of 3 reveals that a perchlorate ion linked to the complex by hydrogen bonding via a water molecule.