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We report Ni II and Cu II complexes of a few pyrrolecarboxamide ligands containing -H, -Cl, and -CH 3 substituents on the phenylene ring. Solid-state X-ray diffraction and solution-based spectral studies substantiated a square-planar geometry around the metal ions in all six of the M II complexes. Electrochemical studies showed that the electronic substituents considerably influence the M 3+/2+ redox potentials. All [a]4957 of the complexes exhibit considerably low M 3+/2+ redox potentials owing to their tetraanionic coordination environments. Chemical and/or electrochemical oxidation has resulted in the isolation of Ni 3+ complexes and the generation of Cu 3+ species. The spectroscopic studies revealed squareplanar geometries around the metal ions in the resultant Ni 3+ and Cu 3+ complexes. 4958cations are involved in C-H···O interactions with O amide atoms to create a chain, whereas lattice N,N-dimethylformamide (DMF) molecules are held in place through C-H···π interactions from arene and pyrrole rings.

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