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However, the practical application of COFs for scalable solar\u2010to\u2010hydrogen conversion remains limited due to their insufficient photocatalytic efficiencies. Herein, we achieved an exceptionally high hydrogen evolution rate of 364\u00a0mmol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    using HCl\u2010protonated COF\u2010920 under ultraviolet\u2010visible light, as confirmed by water\u2010drainage and gas\u2010gathering experiments, exceeding most previously reported COF\u2010based photocatalysts. Three series of isoreticular COFs were synthesized, incorporating benzene, biphenyl, and triphenyl linkers, along with their structural isomers featuring reversed imine bond orientations, to systematically investigate the collaborative influences of linker length, structural isomerism, and protonation on the photocatalytic performance. Experimental results revealed that COFs employing biphenyl\u2010based linkers exhibited superior photocatalytic activity compared to those with benzene or triphenyl linkers. Moreover, the performance difference resulting from variations in imine orientation decreases with increasing linker length, supported by density functional theory (DFT) calculations revealing narrower energy differences between units connected by imine bonds (\u2500C\u2550N\u2500). Our findings not only provide new insights into structure\u2013activity relationships in COF photocatalysts but also highlight the potential of COF materials for sustainable solar\u2010to\u2010fuel conversion.\n                  <\/jats:p>","DOI":"10.1002\/anie.202511200","type":"journal-article","created":{"date-parts":[[2025,6,24]],"date-time":"2025-06-24T12:13:53Z","timestamp":1750767233000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":29,"title":["Synergistic Enhancement of Photocatalytic Hydrogen Evolution in Covalent Organic Frameworks via Isoreticular Design, Isomerism, and Protonation"],"prefix":"10.1002","volume":"64","author":[{"given":"Wenbo","family":"Dong","sequence":"first","affiliation":[{"name":"College of Polymer Science and Engineering Sichuan University  Chengdu 610065 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xingjiang","family":"Yu","sequence":"additional","affiliation":[{"name":"College of Polymer Science and Engineering Sichuan University  Chengdu 610065 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhiying","family":"Qin","sequence":"additional","affiliation":[{"name":"College of Polymer Science and Engineering Sichuan University  Chengdu 610065 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yushuang","family":"Chen","sequence":"additional","affiliation":[{"name":"College of Polymer Science and Engineering Sichuan University  Chengdu 610065 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shijie","family":"Ren","sequence":"additional","affiliation":[{"name":"College of Polymer Science and Engineering Sichuan University  Chengdu 610065 P. R. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,7,2]]},"reference":[{"key":"e_1_2_7_1_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.aaw8775"},{"key":"e_1_2_7_2_1","doi-asserted-by":"publisher","DOI":"10.1038\/nmat2317"},{"key":"e_1_2_7_3_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41586-021-03907-3"},{"key":"e_1_2_7_4_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41929-023-00972-x"},{"key":"e_1_2_7_5_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-021-26817-4"},{"key":"e_1_2_7_6_1","doi-asserted-by":"publisher","DOI":"10.1039\/C8CS00443A"},{"key":"e_1_2_7_7_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.esci.2024.100354"},{"key":"e_1_2_7_8_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41563-019-0591-1"},{"key":"e_1_2_7_9_1","doi-asserted-by":"publisher","DOI":"10.1039\/D4CS00703D"},{"key":"e_1_2_7_10_1","doi-asserted-by":"publisher","DOI":"10.1039\/D0CS00049C"},{"key":"e_1_2_7_11_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.chemrev.9b00550"},{"key":"e_1_2_7_12_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41565-022-01168-3"},{"key":"e_1_2_7_13_1","doi-asserted-by":"publisher","DOI":"10.1039\/D0CS00017E"},{"key":"e_1_2_7_14_1","doi-asserted-by":"publisher","DOI":"10.1021\/acs.accounts.1c00693"},{"key":"e_1_2_7_15_1","doi-asserted-by":"publisher","DOI":"10.1039\/C4SC00016A"},{"key":"e_1_2_7_16_1","doi-asserted-by":"publisher","DOI":"10.1002\/adfm.202401562"},{"key":"e_1_2_7_17_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.202301190"},{"key":"e_1_2_7_18_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202413096"},{"key":"e_1_2_7_19_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41557-018-0141-5"},{"key":"e_1_2_7_20_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.202308251"},{"key":"e_1_2_7_21_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202501869"},{"key":"e_1_2_7_22_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.3c08220"},{"key":"e_1_2_7_23_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-019-10504-6"},{"key":"e_1_2_7_24_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-023-36338-x"},{"key":"e_1_2_7_25_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202104870"},{"key":"e_1_2_7_26_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-025-57166-1"},{"key":"e_1_2_7_27_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-021-27573-1"},{"key":"e_1_2_7_28_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.apcatb.2024.123837"},{"key":"e_1_2_7_29_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.0c00564"},{"key":"e_1_2_7_30_1","first-page":"9752","volume":"142","author":"Ghosh S.","year":"2020","journal-title":"J. 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