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Specifically, three terpyridine\u2010 and quarterpyridine\u2010based trialdehydes were synthesized, and utilized as the starting monomers to polymerize with trimethylpyridinium bromide to yield vinylene\u2010linked iTPy\u2010COF, iTPPy\u2010COF and iQPPy\u2010COF, respectively. Thus constructed donor\u2010acceptor cationic COFs exhibit considerably high visible\u2010light catalytic efficiency for hydrogen peroxide (H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub>) synthesis by the dual\u2010channel mechanisms of oxygen reduction reaction (ORR) and water oxidation reaction (WOR). In pure water and O<jats:sub>2<\/jats:sub> atmosphere, the H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub> production rate (HPR) of iTPPy\u2010COF after 1\u2005h reaction is as high as 7955\u2005\u03bcmol g<jats:sup>\u22121<\/jats:sup> h<jats:sup>\u22121<\/jats:sup>. Even though in air, its HPR value still reaches 6249\u2005\u03bcmol g<jats:sup>\u22121<\/jats:sup> h<jats:sup>\u22121<\/jats:sup>. Moreover, it is found that changing the arm lengths and ratios of pyridine to benzene ring in the frameworks significantly affects the photocatalytic capability. The structure\u2013property relationship is investigated in terms of the variations of electronic structures through the theoretical simulations and measurements of photophysical parameters such as fluorescence lifetimes, photocurrent intensities, and impedances of charge transfer, which offers new insights into the engineering of multipyridine\u2010based cationic COFs for highly efficient H<jats:sub>2<\/jats:sub>O<jats:sub>2<\/jats:sub> photosynthesis.<\/jats:p>","DOI":"10.1002\/anie.202425617","type":"journal-article","created":{"date-parts":[[2025,2,18]],"date-time":"2025-02-18T11:34:44Z","timestamp":1739878484000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":62,"title":["Terpyridine\u2010 and Quarterpyridine\u2010Based Cationic Covalent Organic Frameworks for Visible\u2010Light\u2010Catalytic H<sub>2<\/sub>O<sub>2<\/sub> Synthesis"],"prefix":"10.1002","volume":"64","author":[{"given":"Jun","family":"Zhang","sequence":"first","affiliation":[{"name":"Department of Polymer Science and Materials School of Chemical Engineering Dalian University of Technology  Linggong Rd. 2 Dalian 116024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Fei","family":"Xue","sequence":"additional","affiliation":[{"name":"Department of Polymer Science and Materials School of Chemical Engineering Dalian University of Technology  Linggong Rd. 2 Dalian 116024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0451-1919","authenticated-orcid":false,"given":"Zhonggang","family":"Wang","sequence":"additional","affiliation":[{"name":"Department of Polymer Science and Materials School of Chemical Engineering Dalian University of Technology  Linggong Rd. 2 Dalian 116024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,2,27]]},"reference":[{"key":"e_1_2_9_1_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.checat.2023.100568"},{"key":"e_1_2_9_2_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-020-20823-8"},{"key":"e_1_2_9_3_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.jhazmat.2019.02.009"},{"key":"e_1_2_9_4_1","doi-asserted-by":"publisher","DOI":"10.1016\/j.cattod.2023.114155"},{"key":"e_1_2_9_5_1","doi-asserted-by":"publisher","DOI":"10.1126\/science.aay1844"},{"key":"e_1_2_9_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.200503779"},{"key":"e_1_2_9_7_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202402095"},{"key":"e_1_2_9_8_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202217479"},{"key":"e_1_2_9_9_1","author":"Liu J.-C.","year":"2024","journal-title":"Angew. 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