The chemical and electrochemical syntheses of the zinc (I) and cadmium (II) complexes are carried out on the basis of the tridentate Schiff base (H2L), the condensation product of (2-tosylaminoaniline) N-(2-aminophenyl)-4-methylbenzenesulfunamide with 1-phenyl-3-methyl-4-formylpyrazole-5-thiol. The structures and compositions of the synthesized metallochelates are proved by the data of C, H, and N elemental analyses, IR spectroscopy, and H-1 NMR spectroscopy. X-ray absorption spectroscopy is used to determine the structure of the zinc complex. The binuclear structure of the cadmium complex is confirmed by the X-ray diffraction data (CIF file CCDC no. 1471159). The optical properties of H2L and the zinc and cadmium complexes in dimethyl sulfoxide (DMSO) solutions are studied.