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A unique supramolecular approach of preparing and using a cucurbit[8]uril (Q[8])-based dynamic host–guest assembly for cyanide sensing in and removal from water has been successfully developed. The dicyanovinyl-attached cationic guest (1) was designed as the fluorescent response moiety for the detection of the cyanide anion via a nucleophilic addition reaction in the assist of the Q[8]-based 2:2 quaternary complexes. Furthermore, the reaction of cyanide with 1 further switched the Q[8]-based host–guest assemblies from the 2:2 complexes to the 1:1 supramolecular polymers that precipitate in water. Thus, the macrocyclic-based dynamic host–guest assembly has potential use in applications for solving the problem of toxic anion pollutants present in aqueous environments.