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2‐Ureido‐4[1H]‐pyrimidinone quadruple hydrogen‐bonded assembly 1·1 containing N,N‐dimethylaminophenyl moiety exhibits a sensitive response to fluoride anion and lead cation. Spectroscopic studies reveal that the presence of small amount of fluoride anions and lead cations can easily disassemble and intercalate 2‐ureido‐4[1H]‐pyrimidinone hydrogen‐bonded supramolecular architectures.
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