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However, structural flexibility and solvent\u2010induced degradation often hinder isolating a single tautomeric emission in water. Here, we introduce a\n                    <jats:italic>linker\u2010locking strategy<\/jats:italic>\n                    that rigidifies the flexible metal\u2013organic framework (MOF) MIL\u201053\u2010(OH)\n                    <jats:sub>2<\/jats:sub>\n                    through cooperative stabilization by encapsulated ligands and structural water, forming a stable phase,\n                    <jats:bold>\n                      rigid L@MIL\u201053\u2010(OH)\n                      <jats:sub>2<\/jats:sub>\n                    <\/jats:bold>\n                    . The hydrogen\u2010bonding network among structural water, encapsulated ligands, and the framework stabilizes the pore structure while preserving reversible interconversion between flexible and rigid phases via ligand and water removal or post\u2010encapsulation. This rigidification suppresses particle fragmentation in aqueous media and enables controlled ESIPT behavior. While flexible MIL\u201053\u2010(OH)\n                    <jats:sub>2<\/jats:sub>\n                    exhibits mixed enol and keto emissions due to size\u2010dependent heterogeneity,\n                    <jats:bold>\n                      rigid L@MIL\u201053\u2010(OH)\n                      <jats:sub>2<\/jats:sub>\n                    <\/jats:bold>\n                    displays a single keto emission with prolonged excited\u2010state lifetimes (&gt;14\u00a0ns in D\n                    <jats:sub>2<\/jats:sub>\n                    O vs &lt;5\u00a0ns in H\n                    <jats:sub>2<\/jats:sub>\n                    O) and distinct optical responses in H\n                    <jats:sub>2<\/jats:sub>\n                    O and D\n                    <jats:sub>2<\/jats:sub>\n                    O. Consequently, the pronounced kinetic isotope effect allows\n                    <jats:bold>\n                      rigid L@MIL\u201053\u2010(OH)\n                      <jats:sub>2<\/jats:sub>\n                    <\/jats:bold>\n                    to sensitively detect trace H\n                    <jats:sub>2<\/jats:sub>\n                    O in D\n                    <jats:sub>2<\/jats:sub>\n                    O with high reusability over at least five cycles. This work establishes\n                    <jats:italic>linker locking<\/jats:italic>\n                    as a new strategy for stabilizing flexible MOFs and controlling excited\u2010state processes for aqueous sensing.\n                  <\/jats:p>","DOI":"10.1002\/advs.77856","type":"journal-article","created":{"date-parts":[[2026,9,27]],"date-time":"2026-09-27T18:00:31Z","timestamp":1790532031000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Linker\u2010Locking Strategy for the Rigidification of Flexible Metal\u2013Organic Framework: Structural Stabilization and Controlled ESIPT for H\n                    <sub>2<\/sub>\n                    O\/D\n                    <sub>2<\/sub>\n                    O Sensing"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-7819-2570","authenticated-orcid":false,"given":"Amitosh","family":"Sharma","sequence":"first","affiliation":[{"name":"Department 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