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Here, by subtly modifying one building unit, we synthesized three chemically related imine-linked COFs that span an architectural sequence from layered 2D kgm and 2D sql frameworks to an entangled 3D sql framework. This architectural evolution disrupts extended planar packing, reduces confinement around the imine linkages, and generates an interconnected, water-accessible pore network. Consistent with these architectural features, the entangled 3D COF exhibits a proton conductivity approximately 5 orders of magnitude higher than those of the two layered analogues, despite only a modest increase in total water uptake. Subsequent mild oxidation of imine linkages to amide linkages further enhanced proton transport while largely preserving the crystallinity of the entangled framework. This work demonstrates that architectural evolution can activate the latent functionality of buried polar linkages, providing a design principle for functional porous materials.<\/jats:p>","DOI":"10.1021\/jacs.6c11748","type":"journal-article","created":{"date-parts":[[2026,8,20]],"date-time":"2026-08-20T18:01:28Z","timestamp":1787248888000},"page":"36320-36326","source":"Crossref","is-referenced-by-count":0,"title":["Architectural\nEvolution Unlocks the Functional Potential\nof Buried Sites in Covalent Organic Frameworks"],"prefix":"10.1021","volume":"148","author":[{"given":"Wei-De","family":"Zhu","sequence":"first","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiao-Chun","family":"Lin","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yi-Ling","family":"Zhong","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4137-9005","authenticated-orcid":true,"given":"Hai-Sen","family":"Xu","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiao-Yu","family":"Wu","sequence":"additional","affiliation":[{"name":"Sinopec Shanghai Research Institute of Petrochemical Technology , , ,","place":["Shanghai, China, 200128"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongfei","family":"Wang","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0002-0670-9419","authenticated-orcid":true,"given":"Zhi-Ye","family":"Zhong","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Wen-Na","family":"Jiao","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Si","family":"Huang","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jia-Hao","family":"Chen","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Han","family":"Chen","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6468-2990","authenticated-orcid":true,"given":"Yi","family":"Luo","sequence":"additional","affiliation":[{"name":"Sinopec Shanghai Research Institute of Petrochemical Technology , , ,","place":["Shanghai, China, 200128"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8094-7813","authenticated-orcid":true,"given":"Marcel","family":"Mayor","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3604-7858","authenticated-orcid":true,"given":"Cheng-Yong","family":"Su","sequence":"additional","affiliation":[{"name":"Sun Yat-Sen University , , ,","place":["Guangzhou, China, 510275"]},{"name":"Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences , , ,","place":["Shanghai, China, 200032"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,20]]},"reference":[{"issue":"5751","key":"2026090312084343600_cit1","doi-asserted-by":"publisher","first-page":"1166","DOI":"10.1126\/science.1120411","article-title":"Porous, Crystalline, Covalent Organic\nFrameworks","volume":"310","author":"Co\u0302te\u0301","year":"2005","journal-title":"Science"},{"issue":"13","key":"2026090312084343600_cit2","doi-asserted-by":"publisher","first-page":"4570","DOI":"10.1021\/ja8096256","article-title":"A Crystalline Imine-Linked\n3-D Porous\nCovalent Organic Framework","volume":"131","author":"Uribe-Romo","year":"2009","journal-title":"J. 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