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Herein, we propose a strategy that constrains segmental motion by\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2013\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2010driven ordered stacking. Guided by Random Forest (RF) analysis of substructure marginal contributions, we selected a pre\u2010existing high FFV aromatic substructure (\n                    <jats:italic>p<\/jats:italic>\n                    \u2010terphenyl) and, inspired by articular joints, assembled it into rigid\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2013\n                    <jats:italic>\u03c0<\/jats:italic>\n                    \u2010stacked domains linked by flexible amide units, creating a semi\u2010crystalline membrane (DATP) characterized by short\u2010range order embedded within long\u2010range disorder. Organic\u2010organic interfacial polymerization (OOIP) yields this scalable network, further reducing transport resistance by tuning ordered and disordered domain arrangements. The DATP membrane features rigidly interconnected channels, increasing FFV by 14% to 35.5% compared to the amorphous membrane (DAB), while reducing interconnected volume loss during operation by 14.3%. This achieves a record\u2010high methanol permeability of 2779 L m\n                    <jats:sup>\u22122<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    bar\n                    <jats:sup>\u22121<\/jats:sup>\n                    nm and the highest selectivity among all polymer membranes with comparable molecular weight cut\u2010off (MWCO). Extended to active pharmaceutical ingredients (APIs) separation, it enables 50\u2010fold enrichment within 2.5 h and shows 28% higher selectivity than commercial membranes. By endowing polymer membranes with the structural tunability of crystalline materials, this work combines well\u2010defined pore architecture with scalable fabrication.\n                  <\/jats:p>","DOI":"10.1002\/advs.77001","type":"journal-article","created":{"date-parts":[[2026,8,5]],"date-time":"2026-08-05T13:58:59Z","timestamp":1785938339000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Architecture\u2010Engineered Semi\u2010Crystalline Microporous Polymer Membranes for Precise Molecular Separation"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0008-6643-4342","authenticated-orcid":false,"given":"Zi\u2010Meng","family":"Xu","sequence":"first","affiliation":[{"name":"School of Chemical Engineering and Technology School of Chemistry Southern Marine Science and Engineering Guangdong Laboratory (Zhuhai) OFMMT Sun Yat\u2010sen University  Guangzhou People's Republic of 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Engineering and Technology School of Chemistry Southern Marine Science and Engineering Guangdong Laboratory (Zhuhai) OFMMT Sun Yat\u2010sen University  Guangzhou People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guang\u2010Yong","family":"Shen","sequence":"additional","affiliation":[{"name":"China Lucky Group Corporation  Baoding People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ya\u2010Zhao","family":"Li","sequence":"additional","affiliation":[{"name":"China Lucky Group Corporation  Baoding People's Republic of China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yi","family":"Li","sequence":"additional","affiliation":[{"name":"School of Chemical Engineering and Technology School of Chemistry Southern Marine Science and Engineering Guangdong Laboratory (Zhuhai) OFMMT Sun Yat\u2010sen University  Guangzhou People's Republic of 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