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Herein, [3+3] imine condensation of 1,3,5\u2010trimethyl\u20102,4,6\u2010tris(4\u2010aminophenyl)benzene with 1,3,5\u2010triethyl\u20102,4,6\u2010tris(4\u2010formylphenyl)benzene affords three single\u2010crystal COF isomers composed of\n                    <jats:bold>hcb<\/jats:bold>\n                    nets. Their AB\n                    <jats:bold>hcb<\/jats:bold>\n                    stacking, double [2D+2D], and triple [2D+2D+2D] crossing entangled structures have been resolved by 3D electron diffraction. Among the three desolvated COFs, GZU\u20104a exhibits the highest ethane uptake (100.7 cm\n                    <jats:sup>3<\/jats:sup>\n                    g\n                    <jats:sup>\u22121<\/jats:sup>\n                    ) and ethane\/ethylene selectivity (1.6), enabling one\u2010step production of high\u2010purity ethylene (&gt;99.99%) in dynamic breakthrough experiments. The superior and inverse separation performance originates from its rigid non\u2010interpenetrated framework with optimized pore confinement for strengthened ethane binding. This work not only presents an unprecedented example of triple isomeric COFs with atom\u2010resolution structures from non\u2010interpenetration to inclined interpenetration of 2D nets, but also shows an inverse adsorption selectivity for ethane over ethylene, greatly enriching the diversity of COFs.\n                  <\/jats:p>","DOI":"10.1002\/anie.5362334","type":"journal-article","created":{"date-parts":[[2026,7,29]],"date-time":"2026-07-29T14:23:29Z","timestamp":1785335009000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Triple Framework Isomerism and Efficient Ethane\/Ethylene Separation of Single\u2010Crystal Covalent Organic Frameworks With 2D hcb Sheets"],"prefix":"10.1002","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3379-7581","authenticated-orcid":false,"given":"Baoqiu","family":"Yu","sequence":"first","affiliation":[{"name":"Guizhou Key Laboratory of Macrocyclic and 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University  Guiyang China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qingmei","family":"Xu","sequence":"additional","affiliation":[{"name":"Beijing Key Laboratory for Science and Application of Functional Molecular and Crystalline Materials Department of Chemistry and Chemical Engineering School of Chemistry and Biological Engineering University of Science and Technology Beijing  Beijing China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shangwei","family":"Yuan","sequence":"additional","affiliation":[{"name":"Guizhou Key Laboratory of Macrocyclic and Supramolecular Chemistry School of Chemistry and Chemical Engineering Guizhou University  Guiyang China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6432-2875","authenticated-orcid":false,"given":"Xin","family":"Xiao","sequence":"additional","affiliation":[{"name":"Guizhou Key Laboratory of Macrocyclic and Supramolecular Chemistry School of Chemistry and Chemical Engineering Guizhou University  Guiyang China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xu","family":"Ding","sequence":"additional","affiliation":[{"name":"Guizhou Key Laboratory of Macrocyclic and Supramolecular Chemistry School of Chemistry and Chemical Engineering Guizhou University  Guiyang China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0138-2966","authenticated-orcid":false,"given":"Hailong","family":"Wang","sequence":"additional","affiliation":[{"name":"Beijing Key Laboratory for Science and Application of Functional Molecular and Crystalline Materials Department of Chemistry and Chemical Engineering School of Chemistry and Biological Engineering University of Science and Technology Beijing  Beijing 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numbers 2413077 (for GZU\u20104) 2413079 (for GZU\u20105) and 2413078 (for GZU\u20106) contain the supplementary crystallographic data for this paper. 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