AbstractTwo amide‐imine conjugates where amide is synthesized by reacting hydrazine with 4‐hydroxybenzoic acid and subsequently condensed with 2‐hydroxy naphthalene‐1‐carbaldehyde (m1) and 2‐hydroxy benzaldehyde (m2), selectively detects Mo(VI) at nano molar level via change in emission characteristics. The interactions have been authenticated from single crystal X‐ray structures of resulting Mo(VI) complexes (Mo1 and Mo2). Further, Mo1 selectively interacts with AsO2− via formation of H‐bond that facilitates its detection through change of emission characteristics. The binding constant of Mo1 for AsO2− is 1.02×105 M−1/2. The TCSPC studies support the interaction of Mo1 with AsO2−. The probe‐analyte interaction has also been established by different spectroscopic techniques like 1H NMR, ESI‐MS, FTIR and Jobs experiment. Theoretical DFT studies justifies the reason behind the interaction and support experimental spectroscopic findings. Notably, the sequential fluorescence recognition of Mo(VI) and AsO2− by m1 have been explored to construct a logic gate.
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