Three substituted-pyridyl functionalized bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) derivatives 1-3 and their corresponding Ni(II) and Co(II) complexes have been synthesized and characterized. Their electrochemical properties in CH2Cl2 solution have been investigated by cyclic voltammetry and two reversible single-electron oxidation waves for the TTF moiety are observed. Crystal structure analyses were carried out for compound 2 as well as for the Co(II) complex of 1 (7). © 2007 Elsevier B.V. All rights reserved.