Pale‐green crystals of the title complex were prepared by reaction of 2‐formylpyridine semicarbazone (HCSpy) and nickel(II) perchlorate in boiling ethanol. The crystals are triclinic with the nickel ion in an octahedral arrangement, coordinated by two nitrogen atoms and one oxygen donor atom from each ligand molecule. The effect of coordination on bond lengths and angles was explored by comparison with the single‐crystal structure data of the free ligand HSCpy, which was collected as well. The assumed coordination mode was supported by 1H and 13C NMR spectroscopic data. A detailed analysis of the electronic properties, including semi‐empirical quantummechanical calculations is presented. Furthermore, the data obtained from magnetic susceptibility and EPR measurements are in accordance with a low‐spin d8 nickel(II) complex.

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The pyridine-2-carbaldehyde semicarbazone ligand (HL) reacts with iron(II) and copper(II) perchlorates in boiling ethanol to yield red-violet [Fe II (HL) 2 ](ClO 4 ) 2 · H 2 O (1) and light-green crystals [Cu II (HL) 2 ](ClO 4 ) 2 · H 2 O (2). The crystals are triclinic with the metal ions in an octahedral environment, coordinated to two nitro-1801 gen and one oxygen-donor atom from HL. Electronic, magnetic and electrochemical properties are presented as well.www.zaac.wiley-vch.de 1805 disc electrode and a platinum wire were used as working and auxiliary electrodes, respectively. Potentials were measured against a Ag/AgCl reference electrode (0.22234 V vs SHE).Microanalyses were done at the Instituto de Química-USP, Brazil.

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