Seven new cobalt(II) and nickel(II) complexes with Schiff's bases were synthesized. The Schiff's bases were prepared by the condensation of 1-aminonaphthalene with carbinols, alpha-hydroxy-alpha-phenylacetophenone (L-1), salicylaldehyde (L-2), and 2-hydroxy-1-naphthaldehyde (L-3), and of 2-aminonaphthalenesulfonic-5 acid with 2-hydroxy-1-naphthaldehyde (L-4). The compounds were studied by X-ray powder diffraction, thermogravimetry, measurements of magnetic susceptibility, and spectroscopy (IR and diffuse reflectance). The coordination sites of the ligand and their dentate members were determined. A coordination number of four was realized in the Ni(II) and Co(II) complexes with L-1-L-3, and the complexes with L-4 were characterized by a coordination number of six (a dimer with an octahedral environment of each central ion).