A novel hexanuclear complex [ (CuL)2Cu 2(l-dca)2](ClO4)2 2L0(1) (whereH2L = (OH)C6H4C(CH3)@N(CH2)3- N@C(CH3)C6H4(OH) or N,N0-bis(2-hydroxyacetophenone) propylenediimine and dca = N(CN)2 and L0 = 2- hydroxyacetophenone) has been synthesized and characterized by elemental analysis, UVa??Vis, FT-IR spectroscopic and electrochemical methods. Single crystal X-ray structural characterization reveals a centrosymmetric nature of the complex unit, where the metal centers adopt distorted square-planar and distorted octahedral geometries. Structural analysis also reveals l2-phenoxo bridges between terminal and the central copper(II) centers of the asymmetric [(CuL)2Cu(dca)] unit, the latter being interconnected to its symmetry related counterpart by double l1,5-dca bridges, leading to the hexanuclear complex ion [ (CuL)2Cu 2(l-dca)2]2+. Low temperature susceptibility measurements of 1 revealed the presence of strong antiferromagnetic coupling (2J = 407 cm 1) between the copper(II) centers.