The work in this report presents the syntheses, characterization and crystal structures of [{CuIILop}2(H5O2)](ClO4) (1), [{CuIILhex}2(H5O2)](ClO4) (2) and [{CuIILen}2(H5O2)](ClO4) (3) derived from three 3-ethoxysalicylaldehyde-diamine Schiff base compartmental ligands H2Lop, H2Lhex and H2Len, in which the diimine moieties come from ortho-phenylenediamine, trans-1,2-diaminocyclohexane and ethylenediamine, respectively. Compounds 1 and 2 crystallize in triclinic crystal system having P space group, while the crystal system and space group of compound 3 is monoclinic P21/c. In the [{CuIILop/hex/en}2(H5O2)]+ cation in 1–3, the two OH2 sites of the aquated proton, H5O2+, interact with two O(phenoxo)2O(ethoxy)2 compartments of the two [CuIILop/hex/en] moieties by forming bifurcated hydrogen bonds and thus [{CuIILop/hex/en}2(H5O2)]+ may be considered as a supramolecular dimer of two mononuclear moieties, self-assembled by H5O2+ as the tecton. On the basis of the extent of the difference in the two O–H distances involving the central hydrogen atom, H5O2+ moieties in 1–3 may be considered as H2O+–H⋯OH2 (in 1) or as the resonance hybrid of H2O+–H⋯OH2 and [H2O⋯H⋯OH2]+ (in 2 and 3). A unique aspect in the composition of 1–3 in terms of the interaction of metal complexes with an aquated proton has been discussed.
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