Two novel coordination polymers, Cu-3(4-pyt)(3) (1) and Co(4-pyt)(2) (2) (4-pyt = pyridine-4-thiolate), have been synthesized by in situ generation of a 4-pyt ligand from a 4,4'-dithiodipyridine precursor through reductive cleavage of the disulfide bond under solvothermal conditions. 1 and 2 exhibit a three-dimensional (3,4)-connected network and a two-dimensional square-grid-type structure, respectively.