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Porous materials with open metal sites (OMSs) have been widely employed to separate various gas mixtures; however, routine OMSs often show the limitation in C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    separation due to the comparable binding affinity with the two gases. Herein, we report a new strategy of anchoring highly unsaturated nickel(II) sites into a large\u2010pore MOF (Ni\n                    <jats:sup>2+<\/jats:sup>\n                    @NOTT\u2010101\u2010(COOH)\n                    <jats:sub>2<\/jats:sub>\n                    ) for simultaneously improving C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and selectivity. The coordination geometry of the anchored Ni\n                    <jats:sup>2+<\/jats:sup>\n                    ion was accurately determined by SCXRD studies, featuring a two\u2010coordination model with highly unsaturated OMSs after the activation. This highly unsaturated Ni\n                    <jats:sup>2+<\/jats:sup>\n                    ion can provide additional binding sites to improve C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and also enable highly selective binding of C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    over CO\n                    <jats:sub>2<\/jats:sub>\n                    through the specific and strong \u03c0\u2010 complexation interactions, as revealed by gas\u2010loaded SCXRD studies and theoretical simulations. This metalated MOF thus exhibits both significantly enhanced C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    uptake (201.4 cm\n                    <jats:sup>3<\/jats:sup>\n                    g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) and C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    selectivity (25.7) than the pristine NOTT\u2010101\u2010(COOH)\n                    <jats:sub>2<\/jats:sub>\n                    (148.0 cm\n                    <jats:sup>3<\/jats:sup>\n                    g\n                    <jats:sup>\u22121<\/jats:sup>\n                    and 3.8) at 298\u00a0K and 1\u00a0bar, making an unprecedented balance between C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and selectivity to overcome the trade\u2010off challenge. Breakthrough experiments on equimolar C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    \/CO\n                    <jats:sub>2<\/jats:sub>\n                    mixtures afford both the top\u2010tier dynamic selectivity (14.4) and C\n                    <jats:sub>2<\/jats:sub>\n                    H\n                    <jats:sub>2<\/jats:sub>\n                    productivity of 114.5\u00a0L kg\n                    <jats:sup>\u22121<\/jats:sup>\n                    (&gt;99.5% purity) at ambient conditions.\n                  <\/jats:p>","DOI":"10.1002\/anie.202506055","type":"journal-article","created":{"date-parts":[[2025,4,28]],"date-time":"2025-04-28T12:30:05Z","timestamp":1745843405000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":39,"title":["Anchoring Highly Unsaturated Nickel(II) Sites into a Metal\u2013Organic Framework for Simultaneous High C\n                    <sub>2<\/sub>\n                    H\n                    <sub>2<\/sub>\n                    Adsorption and Separation"],"prefix":"10.1002","volume":"64","author":[{"given":"Yi\u2010Zhan","family":"Hao","sequence":"first","affiliation":[{"name":"State Key Laboratory of Silicon and Advanced Semiconductor Materials School of Materials Science and Engineering Zhejiang University  Hangzhou 310027 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hui\u2010Min","family":"Wen","sequence":"additional","affiliation":[{"name":"College of Chemical Engineering Zhejiang University of Technology  Hangzhou 310014 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yi\u2010Hong","family":"Yu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Silicon and Advanced Semiconductor Materials School of Materials Science and Engineering Zhejiang University  Hangzhou 310027 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Zhejiang Normal University  Jinhua 321004 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bin","family":"Li","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Silicon and Advanced Semiconductor Materials School of Materials Science and Engineering Zhejiang University  Hangzhou 310027 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guodong","family":"Qian","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Silicon and Advanced Semiconductor Materials School of Materials Science and Engineering Zhejiang University  Hangzhou 310027 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