Six copper(II) complexes of tetracoordinating, pyridinyl-containing 14-membered macrocycles with varying ratios of nitrogen and oxygen donor atoms were prepared and characterized by IR, UV/Vis, and EPR spectroscopy and cyclic voltammetry. A distorted tetragonal coordination of the copper center in the solid-state was established by X-ray crystallography for the tetraazamacrocyclic complex Cu-3 carrying a methoxybenzyl pendent arm and the trioxaaza complex Cu-6. The superoxide dismutase-like activity of the Cu II complexes was investigated by inhibition of NADH oxidation. Al-
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