The pyridine‐2‐carbaldehyde semicarbazone ligand (HL) reacts with iron(II) and copper(II) perchlorates in boiling ethanol to yield red‐violet [FeII(HL)2](ClO4)2·H2O ( 1 ) and light‐green crystals [CuII(HL)2](ClO4)2·H2O ( 2 ). The crystals are triclinic with the metal ions in an octahedral environment, coordinated to two nitrogen and one oxygen‐donor atom from HL. Electronic, magnetic and electrochemical properties are presented as well.