A series of organosilicon(IV) and organotin(IV) complexes having the formulae R(2)MCl(L(1)), R(2)MCl(L(2)), R(2)MCl(L(3)), R(2)MCl(L(4)), R(2)M(L(1))(2), R(2)M(L(2))(2), R(2)M(L(3))(2), and R(2)M(L(4))(2), where M = Si and Sn, and R = CH(3), were synthesized with Schiff bases 5-mercapto-4-(pyridine-2-carboxalideneamino)-s-triazole (HL(1)), 4-(furfuralideneamino)-5mercapto-s-triazole (HL(2)), 4-(2-chlorobenzylideneamino)-5-mercapto-s-triazole (HL(3)), and 4-(4-flourobenzylideneamino)-5-mercapto-s-triazole (HL(4)). These complexes were characterized by elemental analysis, molar conductance, and spectroscopic studies, including UV, IR, (1)H, (13)C, (29)Si, and (119)Sn NMR spectroscopy. On the basis of these studies, the resulting complexes are proposed to have trigonal bipyramidal and octahedral geometries.