The design and synthesis of a supramolecular square was achieved by coordination-driven assembly of redox-active nickel(ii) salen linkers and (ethylenediamine)palladium(ii) nodes. The tetrameric geometry of the supramolecular structure was confirmed via MS, NMR, and electrochemical experiments. While oxidation of the monomeric metalloligand Schiff-base affords a Ni(iii) species, oxidation of the coordination-driven assembly results in ligand radical formation.
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