The "one-pot" synthesis and characterization of a large 28-mer macrocycle (H4L2) with oxamido units capable ofcomplexing guest ions through oxygen or nitrogen donor atoms is reported. Single-crystal structure determinationof H8L2(NO3)4 and {Cu2[H2L2](H2O)2}(NO3)2 demonstrated that the macrocycle contains two sites capable ofcomplexing two nitrate anions or two copper(II) ions, involving a large structural reorganization in the conformationof the macrocyclic framework on coordination of the copper(II) ions when compared to the nitrate. Electrochemicaland magnetic susceptibility measurements on the dinuclear Cu(II) complex and the related mononuclear and trinuclearCu(II) complexes derived from the related 14-mer macrocycle were carried out and illustrate the role of the oxamidogroups in mediating metal-metal interaction and delocalization.