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Herein, three new triamino monomers with a central core of pyridine or benzene surrounded by three pyrimidine or pyridine rings are successfully synthesized, and utilized to polycondense with 1,3,5\u2010triformylphloroglucinol, respectively, to obtain three covalent organic frameworks (COFs) with large specific surface areas. Of interest is the observation that the photocatalytic efficiencies are dramatically promoted by elaborately modulating the position and number of electronegative nitrogen atoms in the N\u2010heterocyclic building blocks of COF frameworks. Under the visible light catalysis, the benzene\u2010cored multipyrimidine COF exhibits the H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production rates of 10762\u00a0\u00b5mol g\n                    <jats:sup>\u22121\u00a0<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    (in water\/O\n                    <jats:sub>2<\/jats:sub>\n                    ) and 9613\u00a0\u00b5mol g\n                    <jats:sup>\u22121\u00a0<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    (in water\/air) at the reaction time of 1\u00a0h without the assistance of any sacrificial agent, representing the highest values among the photocatalysts already reported in the literature under the similar condition. The structure\u2010property relationships and photocatalytic mechanism are studied by virtue of a series of controlled experiments and theoretical calculations, which provide new understanding on the molecular engineering of nitrogen\u2010rich COFs for highly efficient H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    photosynthesis.\n                  <\/jats:p>","DOI":"10.1002\/smll.202507052","type":"journal-article","created":{"date-parts":[[2025,7,21]],"date-time":"2025-07-21T06:23:25Z","timestamp":1753079005000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":7,"title":["Nitrogen Modulation in Multipyrimidine\u2010 and Multipyridine\u2010Based Covalent Organic Frameworks with Exceptional Promotion for Photocatalytic H\n                    <sub>2<\/sub>\n                    O\n                    <sub>2<\/sub>\n                    Synthesis"],"prefix":"10.1002","volume":"21","author":[{"given":"Jun","family":"Zhang","sequence":"first","affiliation":[{"name":"Department of Polymer Science and Materials School of Chemical Engineering Dalian University of Technology  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  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  Dalian 116024 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