The reaction of the Tc(I) complex [Tc(NO)Cl-2(HOMe)(PPh3)(2)] with stoichiometric amounts of 2-mercatopyridine and a proton scavenger yields [Tc(NO)Cl(Spy)(PPh3)(2)] or [Tc(NO)(Spy)(2)(PPh3)], depending upon quantities of ligands employed. These two complexes have been structurally characterized. The small bite angles of the bidentate mercaptopyridine ligands cause significant deviation from octahedral coordination geometry. (C) 2010 Elsevier B.V. All rights reserved.