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A new electrochemical sensor of metal cation in an aqueous solution based on homobifunctional tridentate disulfide Schiff base and named 1,1'-(-((disulfanediylbis(2,1-phenylene))bis(azaneylylidene))bis(methaneylylidene))bis(naphthalene-2-ol) (ATNA) was easily obtained quantitatively from the condensation reaction of 2-hydroxy-1-naphthaldehyde and2-aminothiophenol, and then fully characterized by spectroscopic techniques for structure elucidation. The molecular structure of ATNA was also confirmed by a single-crystal X-ray diffraction st