Preparation and chemical analysis of Mn(II), Fe(III), Co(II), Ni(II), and Zn(II) complexes with Schiff base L [o-HOC6H4CH:N(CH2)6N:CHC6H4OH-o] are the main tasks of this work. The octahedral (M2L2·nH2O·X) complexes in 1 : 1 M : L ratio (X = NO3− or Ac− group, L = ligand) were prepared by involving the hydroxylic group in ortho position. All complexes were characterized on the basis of elemental analysis, UV, IR, 1H NMR, Gc/Ms, thermogravimetric analysis, magnetic measurements, molar conductance, and electrical conductivity. The obtained data indicate that all the investigated compounds behave as semiconductor materials.