6,6'-Methylenebis-[1,11-di(hydroximino)2,3 :9,10-dibenzo-4,8-dioxaundecane], (H4L) 4 was prepared by the reaction of 6,6'-methylenebis-(5'-on-3',4'-benzo-2'-oxapentyl)-1,11-dion-2,3:9,10-dibenzo-4,8-dioxaundecane, 3 with hydroxylamine hydrochloride. Di-and tetranuclear copper(I) and (II) complexes with a bistetradentate ligand, (LH4) have been prepared and identified by a combination of elemental analysis, C-13, H-1-NMR, mass spectra, magnetic moments, IR, UV/Vis, and ESR spectral studies. A geometric optimization of the synthesized ligand 4 was made by the method of molecular mechanics (MM2) in order to establish a stable conformation. The total energy for these conformations are calculated to be 10.94 and 9.49 kcal/mol. (C) 1997 Elsevier Science Ltd.