Lanthanide metal–organic frameworks (Ln-MOFs) have unique advantages in sensing due to their excellent optical properties. In this study, we synthesized a dicarboxylic acid ligand with amide groups and successfully synthesized a novel two-dimensional (2D) MOF with the molecular formula C42H31EuN4O10 (Eu-MOF) by a solvothermal method. Single-crystal X-ray diffraction showed that amide groups are exposed on the outside of the two-dimensional coordination layer, with the possibility of recognizing specific molecules through hydrogen bonding interactions. The ligand’s “antenna effect” enables Eu-MOF to emit a strong luminescence characterized by the “f–f” transition. Further studies have revealed that Eu-MOF could be used as a bifunctional fluorescent probe for the selective detection of benzaldehyde and Fe3+. The sensing mechanism has been analyzed in detail through powder X-ray diffraction (PXRD) analysis, UV-vis spectroscopy, fluorescence lifetime measurement, and density functional (DFT) theory calculation. This design and research can provide a reference for subsequent related work.
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