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Here, we report a dual locking strategy in an aluminum\u2013pyrrolic framework (Al\u2010PyDC) with V\u2010shaped ligand featured AlO\n                    <jats:sub>6<\/jats:sub>\n                    chains and pyrrole dual recognition sites that simultaneously stabilize the V\u2010shaped\n                    <jats:italic>meta<\/jats:italic>\n                    \u2010xylene (mX). This dual\u2010locking effect promotes dense packing of mX within confined channels, resulting in a high adsorption capacity for mX (4.0\u00a0mmol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ), which is much higher than that for\n                    <jats:italic>ortho<\/jats:italic>\n                    \u2010xylene (oX, 2.5\u00a0mmol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) and\n                    <jats:italic>para<\/jats:italic>\n                    \u2010xylene (pX, 2.0\u00a0mmol\u00a0g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ). The simulations and solid\u2010state NMR spectroscopy further confirmed that mX experienced stronger locking interactions with the AlO\n                    <jats:sub>6<\/jats:sub>\n                    chains and pyrrolic ligands compared to pX. Notably, the dual locking effect was temperature\u2010dependent, and elevated temperature accelerated molecular diffusion, thereby weakening the effectiveness of the recognition. Hence, Al\u2010PyDC achieved an excellent mX\/pX selectivity of 8.0 in vapor\u2010phase breakthrough measurements at ambient temperature (303\u00a0K), which outperformed most of the MOF counterparts. Additionally, the isomorphic CAU\u201010\u2010H with V\u2010shaped AlO\n                    <jats:sub>6<\/jats:sub>\n                    \u2013phenyl\u2013AlO\n                    <jats:sub>6<\/jats:sub>\n                    dual locking sites was employed as a control material to elucidate the role of active\u2010site in molecular recognition. This dual locking strategy offered an effective approach for enhancing the adsorption capacity and selectivity for challenging isomer separations.\n                  <\/jats:p>","DOI":"10.1002\/anie.4842714","type":"journal-article","created":{"date-parts":[[2026,9,3]],"date-time":"2026-09-03T12:55:01Z","timestamp":1788440101000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["A Dual Locking Strategy Enables Highly Selective\n                    <i>meta<\/i>\n                    \u2010Xylene Separation With an Aluminum\u2010Pyrrolic Framework"],"prefix":"10.1002","volume":"65","author":[{"given":"Wen\u2010Qi","family":"Tang","sequence":"first","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal University  Nanjing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wang","family":"Li","sequence":"additional","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal University  Nanjing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Han\u2010Xi","family":"Guan","sequence":"additional","affiliation":[{"name":"Institute of Zhejiang University\u2010Quzhou  Quzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cheng\u2010Yu","family":"Rong","sequence":"additional","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal University  Nanjing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wen\u2010Chu","family":"Huang","sequence":"additional","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal University  Nanjing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xu","family":"Gao","sequence":"additional","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal University  Nanjing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yu","family":"Qi","sequence":"additional","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal University  Nanjing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming","family":"Xu","sequence":"additional","affiliation":[{"name":"Jiangsu Key Laboratory of Micro\u2010Nano Sensing and Separation Science For Analytical Chemistry Jiangsu Key Laboratory of Biofunctional Materials Jiangsu Collaborative Innovation Center of Biomedical Functional Materials, Jiangsu Key Laboratory of New Power Batteries, College of Chemistry and Materials Science, State Key Laboratory of Analytical Chemistry For Life Science, State Key Laboratory of Microbial Technology Nanjing Normal 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