New compartmental macroacyclic and macrocyclic Schiff bases have been prepared by reaction of the formyl precursors 2,3-dihydroxy-benzaldehyde, 3-methoxy-2-hydroxy-benzaldehyde and 2,6-diformyl-4-chlorophenol with 1,2-diaminoethane, 1,3-diaminopropane and the polyethyleneoxy-diamine H 2N(CH 2) 2[O(CH 2) 2] nNH 2 ( n = 1, 2, 3) also with the presence of a templating ion. In these ligands the shape of one or borh compartments has progressively been enlarged and the denticity increased in order to link up to four metal ions into the coordination moiety. These ligands react with copper(II), nickel(II) or lanthanide(III) salts to form mononuclear, homo- and heterodinuclear, homotrinuclear or homotetranuclear complexes. The ligands and the complexes were characterized by elemental analysis, IR, 1H and 13C NMR, mass spectrometry, magnetic susceptibility and SEM investigations.