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Two new nano particles of copper (II) and nickel (II) complexes, [Cu(cd5Clsalen)] (1) and [Ni(cd5Clsalen)] (2) with unsymmetrical tetradentate Schiff base ligand cd5Clsalen={methyl-2-[N-[2-(2-hydroxy-5-choloro-2phenyl) methylidynetrilo]ethyl}amino-1-cyclopentenedithiocarboxylate, were synthesized by hydrothermal method. These compounds were characterized by a variety of physic-chemical techniques via. scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (IR) and elemental analysis. The complexes (in bulk) have a NNOS coordination sphere, with the two nitrogens coordinated in a cis configuration. The coordination around nickel center is essentially square-planar with a small tetrahedral distortion and the geometry around the copper center is square planar. Nano-particles of Copper (II) and Nickel (II) oxides have been prepared by calcination of two different Copper (II) and Nickel (II) complexes at 450 ºC that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and IR spectroscopy. The average size of the particles was estimated from the Sherrer formula. This study demonstrates the Schiff base complexes may be suitable precursors for the preparation of nanoscale materials with different and interesting morphologies.