Thiosemicarbazone derivatives, R-C6H4-CH=N-N=(C-S-C2H5)-NH2 . HBr [R = H (L), (CH3)(2)N (L')], were prepared by a modified general method. Complexes of Cu(I), Zn(II), Cd(II), Hg(II) chloride salts with ligands L and L' were isolated in two different solvents, and have the following stoichiometries: [Hg(L)Cl-2](x) prepared in CH2Cl2 and [Zn(L)Cl-2]. 2H(2)O, [Cd(L)Cl-2](2) . CdCl2 . C2H5OH . 4H(2)O, [Hg(L)Cl-2]. 1/2C(2)H(5)OH, [Cu(L)Cl-2](x), [Cd(L')Cl-2]. CdCl2 . C2H5OH . 2H(2)O, [Hg(L' HBr)]Cl-2 prepared in absolute ethanol. The complexes were characterized by analytical data, UV, IR and H-1 NMR spectroscopy.