Group 12 metal ion complexes of mixed N,S donor ligands N-(2-mercaptoethyl) picolylamine (L) and N-(2-pyridylmethyl)-N-(2-(methylthio)ethyl)-N-(2-thioethyl)-amine (L\u27) were studied. Characterization of the known complex ion [Zn(ZnL2)2]2+ was complemented by X-ray crystallography of a new acetonitrile solvate of the perchlorate salt, ESI-MS and variable temperature NMR studies. In addition, five solvates of the novel alkylthiolate bridged mixed metal complex [Hg(ZnL2)2](ClO4)2 were formed through either indirect and direct methods. Further characterization of the mixed metal complexes was done through variable temperature NMR, ESI-MS and X-ray crystallography. In addition, an unusual bicyclo spiro [5.5] complex with formula [Zn((ZnL\u27)2(m-OH))2](ClO4)4 was prepared and characterized by X-ray crystallography. Characterization of this complex in acetonitrile solution by variable temperature NMR and ESI-MS studies indicated possible formation of a (ZnL¢)4+4 macrocycle as observed for Hg(II) with L\u27, but no evidence for the carbonate complexes formed by Cd(II) with L\u27
