Abstract: | Synthesis, characterization, and X-ray crystal structure for a mixed-valence binuclear Co(II)/Co(III) complex with the dianionic dithiolate form of a pentadentate ligand 2,6-diacetylpyridinebis(thiosemicarbazone) are reported. A new synthetic methodology has been employed replacing usual cobalt(II) salts by [Co(NH3)5Cl]Cl2 as a precursor. The coordination geometry of cobalt(II), CoN2S2, was found to be distorted tetrahedral, whereas the cobalt(III) coordination sphere, CoN4S2, is slightly distorted octahedral. The magnetic behavior and molar conductivity of the complex are in agreement with the mixed-valence state. |