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[Graphical Abstract] As few as 23 enzyme molecules could be detected on the basis of the dispersion of Au nanoparticles in a model bioassay whose sensitivity was boosted by the interplay between multivalent and monovalent supramolecular interactions: a diferrocenyl ligand (red) caused the assembly of nanoparticle clusters; upon its oxidation, a competing monovalent guest molecule (blue) favored the formation of monovalent interactions for more efficient disassembly.