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Conventional generation of\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    relies on metal\u2010containing sensitizers to promote intersystem crossing (ISC) and thereby activate molecular oxygen (\n                    <jats:sup>3<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    ), which limits biocompatibility and scalability. Here, we report a metal\u2010free strategy leveraging excited\u2010state intramolecular\u2010proton\u2010transfer (ESIPT) to enhance\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production. Two classes of ESIPT\u2010active materials, 1D polymers and 2D covalent organic frameworks (COFs), were systematically compared. Interestingly, while the ESIPT transition in the 1D polymer is incomplete and unstable, 2D COF enables a highly stabilized tautomeric transition, resulting in a persistent metastable state that acts as a gateway to enhanced ISC. This difference is due to a reversed ESIPT pathway dictated by ground\u2010state geometry. Time\u2010resolved spectroscopic studies reveal that the ESIPT transition process in the 2D COF triggers ISC, facilitating\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    generation. Thermodynamic analysis reduces the singlet\u2013triplet energy gap and increases dipole moment changes, while spin\u2013orbit coupling and frontier molecular orbital reorganization indicate kinetic facilitation of ISC. This work highlights the unique advantages of 2D\u2010COF\u2010based ESIPT transformations, offering a groundbreaking approach to boosting ISC efficiency and\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    generation, expanding the scope of ESIPT in photocatalytic applications.\n                  <\/jats:p>","DOI":"10.1002\/anie.202515898","type":"journal-article","created":{"date-parts":[[2025,10,14]],"date-time":"2025-10-14T05:43:23Z","timestamp":1760420603000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":35,"title":["Metal\u2010Free Singlet Oxygen Generation via Excited\u2010State Intramolecular Proton\u2010Transfer\u2010Driven Intersystem Crossing in 2D Covalent Organic Frameworks"],"prefix":"10.1002","volume":"64","author":[{"given":"Junyi","family":"Qiu","sequence":"first","affiliation":[{"name":"Laboratory of Solar Fuel Faculty of Materials Science and Chemistry China University of Geosciences  68 Jincheng Street Wuhan 430078 P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chang","family":"Cheng","sequence":"additional","affiliation":[{"name":"Laboratory of Solar Fuel Faculty of Materials Science and Chemistry China University of Geosciences  68 Jincheng Street Wuhan 430078 P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hermenegildo","family":"Garc\u00eda","sequence":"additional","affiliation":[{"name":"Instituto de Tecnolog\u00eda Qu\u00edmica Consejo Superior de Investigaciones Cient\u00edficas\u2010Universitat Polit\u00e8cnica de Valencia Universitat Polit\u00e8cnica de Valencia  Av. De los Naranjos s\/n Valencia 46022 Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guijie","family":"Liang","sequence":"additional","affiliation":[{"name":"Hubei Key Laboratory of Low Dimensional Optoelectronic Materials and Devices Hubei University of Arts and Science  Xiangyang 441053 P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bicheng","family":"Zhu","sequence":"additional","affiliation":[{"name":"Laboratory of Solar Fuel Faculty of Materials Science and Chemistry China University of Geosciences  68 Jincheng Street Wuhan 430078 P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liuyang","family":"Zhang","sequence":"additional","affiliation":[{"name":"Laboratory of Solar Fuel Faculty of Materials Science and Chemistry China University of Geosciences  68 Jincheng Street Wuhan 430078 P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0612-8633","authenticated-orcid":false,"given":"Jiaguo","family":"Yu","sequence":"additional","affiliation":[{"name":"Laboratory of Solar Fuel Faculty of Materials Science and Chemistry China University of Geosciences  68 Jincheng Street Wuhan 430078 P.R. 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