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Inspired by the biological concept of \u201cselection pressure,\u201d we propose that the harshness of synthetic conditions serves as a key selection pressure governing the final state of COFs. A model COFs system comprising flexible tetrazine and rigid pyrene units is designed, and differential selection pressures are applied by adjusting reaction temperature. Under conditions of lower temperature (lower selection pressure), flexible conformations based on non\u2010covalent interactions are preserved, yielding a metastable AA\u2010stacking material (Tz\u2010COF\u2010AA) with high flexibility and environmental sensitivity, which could further transform into an interlayer\u2010shifted phase (Tz\u2010COF\u2010AA'). Under conditions of higher temperature (higher selection pressure), these flexible conformations are disrupted; the system generates a rigid AB\u2010stacking stable material (Tz\u2010COF\u2010AB) dominated by covalent bonds. Iodine adsorption experiments demonstrated that the metastable materials exhibited variability in adsorption performance due to framework flexibility, whereas the stable material possessed performance reproducibility. This selection pressure strategy provides a new example for the controllable construction of metastable COFs and offers insights for the development of porous crystalline materials with tailored dynamic behavior or high stability.<\/jats:p>","DOI":"10.1002\/smll.76249","type":"journal-article","created":{"date-parts":[[2026,10,13]],"date-time":"2026-10-13T09:18:51Z","timestamp":1791883131000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Metastable and Stable States in Covalent Organic Frameworks Controlled by Synthetic Selection Pressure"],"prefix":"10.1002","author":[{"given":"Ziqian","family":"Han","sequence":"first","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yingsi","family":"Huo","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemistry for NBC Hazards Protection Frontiers Science Center for Rare Isotopes School of Nuclear Science and Technology Lanzhou University  Lanzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kaifu","family":"Yu","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Mengyao","family":"Wen","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Honghan","family":"Long","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0008-7922-6366","authenticated-orcid":false,"given":"Jie","family":"Zhang","sequence":"additional","affiliation":[{"name":"NHC Key Laboratory of Nuclear Technology Medical Transformation Mianyang Central Hospital  Mianyang China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0009-5748-3852","authenticated-orcid":false,"given":"Kang","family":"Kang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemistry for NBC Hazards Protection Frontiers Science Center for Rare Isotopes School of Nuclear Science and Technology Lanzhou University  Lanzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2940-6173","authenticated-orcid":false,"given":"Yang","family":"Li","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6317-6287","authenticated-orcid":false,"given":"Lijian","family":"Ma","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,10,13]]},"reference":[{"issue":"5751","key":"e_1_2_9_2_1","doi-asserted-by":"crossref","first-page":"1166","DOI":"10.1126\/science.1120411","article-title":"Porous, Crystalline, Covalent Organic Frameworks","volume":"310","author":"C\u00f4t\u00e9 A. 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