The [Co(XSalen)(PEt 3 )(H 2 O)]ClO 4 , ( X = H, MeO, Br, NO 2 ) , ( where Salen = bi ( salicylaldehyde) 1,2-ethylenediimine) complexes were synthesiszed and characterized by FT-IR, UV-Vis, 1 H NMR, 13 C NMR and 31 P NMR. The coordination geometry of the synthezised complex [Co(5-BrSalen)(PEt 3 )(H 2 O)]ClO 4 was determined by X-ray crystallography. Cobalt(III) Complex has six-coordinated pseudo-octahedral geometry in which the O(1), O(2), N(1) and N(2) atoms of the Schiff base forms the equatorial plane. The spectroscopic and elrctrochemical properties of the complexes were investigated. The electrochemical study of the complexes show that, the reduction of Co(III) is related to the Schiff base ligand. The obtained complexes [Co(Salen)(PEt 3 )(H 2 O)]ClO 4 , [Co(5-NO 2 Salen)(PEt 3 )(H 2 O)]ClO 4 and [Co(Salen)(PBu 3 )(H 2 O)]ClO 4 were incorporated onto the Montmorillonite-K10 nanoclay via simple ion-exchange reaction. The structure and morphology of the obtained nanohybrids were identified by FT-IR, XRD, TGA/DTG, SEM and TEM techniques. Base on the XRD results of the new nano materials, the Schiff base complexes absorbed on outerlayer spaces of clay.
