The reaction of Cu(ClO 4 ) 2 · 6H 2 O and Cd(ClO 4 ) 2 with di-(2-picolyl)sulfur (dps) leads to the formation of mononuclear complexes [Cu(dps)(H 2 O)(ClO 4 )](ClO 4 ) (1) and [Cd(dps) 2 ](ClO 4 ) 2 (2). The crystal structure of 1 exhibits a distorted square pyramidal geometry, coordinated by one sulfur and two nitrogen atoms from the dps ligand, one water molecule and one perchlorate oxygen atom. For 2, the environment around cadmium atom is in a distorted octahedron with four nitrogen and two sulfur atoms from the dps ligand. Cyclic voltammetric data show that complexes undergo two waves of a one-electron transfer corresponding to M(II)/M(III) and M(II)/M(I) processes. Spectral and electrochemical behaviors of the complexes are also discussed.
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