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This paper has selected dicyclohexanocucurbit[6]uril (CyH2Q[6]) as the host and 2-phenylbenzimidazole (G) as the guest to investigate the host–guest interaction mode between CyH2Q[6] and G. Under acidic conditions, the complex was characterized using nuclear magnetic resonance, ultraviolet and fluorescence spectroscopy. The results show that the molecular ratio of CyH2Q[6] to G is 2 : 1. The crystals were cultured with ZnCl2 as a structural inducer under acidic conditions and single crystal X-ray diffraction showed that the molecular ratio of CyH2Q[6] to G is 1 : 3. The G@CyH2Q[6] was used as a fluorescent probe to identify metal cations. The probe exhibits a good selective recognition effect toward Fe3+ ions, which involves a reduced fluorescence intensity with a limit of detection of 1.321 × 10–6 mol l–1.