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We report two isostructural MOFs (NKMOF\u20108\u2010Br and NKMOF\u20108\u2010Me) with ultra\u2010micropores (\u223c6\u00a0\u00c5) integrating bromine\/methyl and cyano groups, creating biomimetic hydrophobic\u2010polar microenvironments for efficient Xe\/Kr separation and nuclear off\u2010gas capture. These MOFs exhibit record low\u2010pressure Xe uptake and Xe packing density. Breakthrough tests under two industrial scenarios\u2014air\u2010separation byproduct purification and trace gas capture\u2014demonstrate unprecedented Kr productivity (12.26\u00a0mmol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) and Xe\/Kr capture capacity (Xe: 32.13\u00a0mmol\u00a0kg\n                    <jats:sup>\u22121<\/jats:sup>\n                    ; Kr: 9.35\u00a0mmol\u00a0kg\n                    <jats:sup>\u22121<\/jats:sup>\n                    ), with retained performance after 500\u00a0kGy\n                    <jats:italic>\u03b2<\/jats:italic>\n                    \u2010irradiation. Single\u2010crystal X\u2010ray diffraction confirms gas molecules preferentially occupying channel centers, stabilized by hydrophobic van der Waals interactions and cyano polarization effects, while theoretical simulations establish a clear structure\u2010property relationship. These results highlight NKMOF\u20108\u2010Br and NKMOF\u20108\u2010Me as leading candidates for energy\u2010efficient noble gas separation and nuclear waste management, and demonstrate a generalizable strategy for engineering adsorption through hydrophobic\u2010polar synergy.\n                  <\/jats:p>","DOI":"10.1002\/anie.202520094","type":"journal-article","created":{"date-parts":[[2025,10,30]],"date-time":"2025-10-30T13:53:19Z","timestamp":1761832399000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":15,"title":["Biomimetic Hydrophobic\u2010Polar Metal\u2010Organic Frameworks for Record\u2010Breaking Separation and Capture of Xenon and Krypton"],"prefix":"10.1002","volume":"64","author":[{"given":"Yizhou","family":"Liu","sequence":"first","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education College of Chemical and Biological Engineering Zhejiang University  Hangzhou Zhejiang 310058 P.R. 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