The reaction of 5-methoxy-5,6-diphenyl-4,5-dihydro-2H-[1,2,4]triazine-3-thione (LH2OCH3)-H-1 with copper(II) chloride leads to the formation of an organic molecule L-2 containing two triazine rings linked by a new S-S bond. A binuclear copper(II) complex, 1, containing L-1 is also isolated. The reaction of (LH2OCH3)-H-1 with copper(l) chloride yields a hexanuclear cluster of copper(l), 2, in which the copper atoms form a distorted octahedron with the ligand L-1 acting as an NS chelate and sulfur bridge, giving to the copper ion a trigonal geometry by one N and two S atoms. In any reaction of the disulfide L-2 with metal salts, complexes containing this molecule are isolated. Reactions with copper(l) and copper(II) chloride and nickel(II) and cadmium(II) nitrate produce the S-S bond cleavage, giving complexes containing the triazine L-1 behaving as the NS anion, which show spectroscopic characteristics identical with those formed by reaction with (LH2OCH3)-H-1. However, the reaction with cobalt(II) nitrate gives a low-spin octahedral cobalt(III) complex, in which an asymmetric rupture of the disulfide L-2 has been produced, giving an unexpected complex with a new ligand and keeping the S-S bond.