We have reported the synthesis and structural characterization of a unique Zn(II) metallacycle (1) and its utilization as a fluorescent probe for the shape-specific selective recognition (turn-off) of Fe and IO ions. The relevant Stern-Volmer graphs indicate that the recognitions of Fe and IO ions are examples of diphasic and monophasic quenchings, respectively. The title metallacycle has been prepared by the reaction of a novel N-heterocyclic carbene precursor, 1,3-bis(2,6-diisopropyl-4-(pyridin-4-yl)phenyl)-1H-imidazol-3-ium chloride/bromide (L), and zinc(II) chloride salt. Notably, the ligand itself did not show any type of recognition for any ions. DFT calculations were performed on L and metallacycle 1 using the geometric parameters, obtained from their single-crystal X-ray diffraction data, to understand the electronic structures of the ligand and macrocycle. The detection limit for the recognition of the Fe ion was determined to be 2.5 × 10 mol/L, and that for IO ion was found to be 6.3 × 10 mol/L.

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