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Here, nitrogen\u2010enriched carbon molecular sieve (CMS) membranes were fabricated from triazine\u2010crosslinked fluorene\u2010based copolyimide precursors. Pendant carboxyl sites enabled triazine crosslinking and anchored nitrogen\u2010rich moieties within the precursor matrix. During pyrolysis, pre\u2010dispersed triazine units carbonized with the polymer backbone, contributing to the formation of pyridinic\u2010N and pyrrolic\u2010N active sites while narrowing ultramicropores to approximately 4.79\u00a0\u00c5. The optimized CL\u2010CMS membrane exhibited a C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    permeability of 4353.0 Barrer, a C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    \/n\u2010C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>10<\/jats:sub>\n                    selectivity of 141.9, and a C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    \/i\u2010C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>10<\/jats:sub>\n                    selectivity of 1817.2, surpassing current upper bounds. Mechanistic analysis revealed a synergistic interplay between nitrogen\u2010enriched pore chemistry and tailored ultramicropore confinement: the former preferentially enhanced C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    affinity, while the latter dominated molecular discrimination through diffusion\u2010controlled sieving, increasing sorption and diffusion selectivities by up to 35% and 97%, respectively. This work establishes triazine\u2010crosslinking\u2010assisted precursor design as a promising strategy to couple adsorption chemistry with ultramicropore architecture, highlighting its potential for highly selective C\n                    <jats:sub>4<\/jats:sub>\n                    separation and polymer\u2010grade C\n                    <jats:sub>4<\/jats:sub>\n                    H\n                    <jats:sub>6<\/jats:sub>\n                    purification.\n                  <\/jats:p>","DOI":"10.1002\/anie.3566490","type":"journal-article","created":{"date-parts":[[2026,9,10]],"date-time":"2026-09-10T08:26:39Z","timestamp":1789028799000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Triazine Crosslinking Enables Nitrogen\u2010Enriched Carbon Molecular Sieve Membranes for Precision 1,3\u2010Butadiene\/n\u2010Butane Separation"],"prefix":"10.1002","author":[{"given":"Fangxu","family":"Fan","sequence":"first","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontier Science Center For Smart Materials School of Chemical Engineering Dalian University of Technology  Dalian Liaoning China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zeyuan","family":"Gao","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontier Science Center For Smart Materials School of Chemical Engineering Dalian University of Technology  Dalian Liaoning China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tianyou","family":"Li","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Fine Chemicals Frontier Science Center For Smart Materials School of Chemical Engineering Dalian University of Technology  Dalian Liaoning 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