A new hydrazone, Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate(C9H11N3O2; Hpyec) and its metal complexes bis(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) nickel(II) monohydrate, [Ni(pyec)2]•H2O (1) and bis(acetato)(Z-ethyl 2-(pyridine-2yl-methylene) hydrazine carboxylate) cadmium (II), [Cd(Hpyec)(CH3COO)2](2), have been prepared by mechano-chemical syntheses and characterized by elemental analysis, UV-visible, IR and NMR spectroscopy, TG-DTA, and solid state emission techniques. The X-ray single crystal structures of both complexes were determined: in 1, the Ni 2+ ion is coordinated by two N, N, O-tridentate anionic ligands to generate a distorted cis-NiO2N4 octahedron. In 2, the cadmium atom is sevencoordinated by one neutral N,N.O-tridentate ligand and two chelating acetate ions to generate a very-distorted CdN2O5 pentagonal bipyramid with the Hpyec atoms occupying both axial and