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Here, we show that a locally flexible pore aperture can act as a kinetic valve that converts the temperature at which a guest is loaded into the temperature at which it is later released. In a pentoxy\u2010functionalized isoreticular MOF (C\n                    <jats:sub>5<\/jats:sub>\n                    \u2010IRMOF), long alkoxy side chains line the aperture to form a strongly confined, thermally responsive gate while preserving a large internal cavity. Unlike its butoxy analogue (C\n                    <jats:sub>4<\/jats:sub>\n                    \u2010IRMOF), a conventional microporous adsorbent, C\n                    <jats:sub>5<\/jats:sub>\n                    \u2010IRMOF traps guests until thermally activated chain motions reopen the gate, releasing them abruptly at an unusually high temperature without any strong binding sites. Cryogenic thermal desorption spectroscopy reveals that the release maximum shifts with a near\u2010unity slope with respect to the initial exposure temperature, defining adsorption\u2010temperature\u2010programmed desorption as a distinct mode of pore function, while the same confinement enables kinetic quantum sieving of hydrogen isotopes up to 100 K. These results establish locally flexible side chains as a simple design handle for programming guest release in porous materials.\n                  <\/jats:p>","DOI":"10.1002\/anie.2943024","type":"journal-article","created":{"date-parts":[[2026,10,7]],"date-time":"2026-10-07T06:44:56Z","timestamp":1791355496000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["A Locally Flexible Kinetic Valve for Temperature\u2010Programmed Guest Release and Hydrogen Isotope Separation in Metal\u2013Organic Frameworks"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-0642-351X","authenticated-orcid":false,"given":"Junsu","family":"Ha","sequence":"first","affiliation":[{"name":"Department of Chemistry and Nanoscience Ewha Womans University  Seoul Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Minji","family":"Jung","sequence":"additional","affiliation":[{"name":"Department 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Daegu Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jihyun","family":"Park","sequence":"additional","affiliation":[{"name":"Department of Chemistry and Nanoscience Ewha Womans University  Seoul Republic of Korea"},{"name":"Institute for Multiscale Matter and Systems Ewha Womans University Seoul Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hyunlim","family":"Kim","sequence":"additional","affiliation":[{"name":"Department of Chemistry Ulsan National Institute of Science and Technology (UNIST)  Ulsan Republic of Korea"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jungwon","family":"Yi","sequence":"additional","affiliation":[{"name":"Department of Chemistry Ulsan National Institute of Science and Technology (UNIST)  Ulsan Republic of 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