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A primary limitation stems from the coupled proton\u2013electron transfer in the two\u2010electron oxygen reduction reaction (2e\n \u2212<\/jats:sup>\n ORR), which demands photoinduced charge generation and rapid proton delivery\u2014features rarely optimized simultaneously in existing COF architectures. Here we address these bottlenecks by combining nanoscale morphological control with pore\u2010wall functionalization. Bottom\u2010up colloidal synthesis produces highly crystalline COF nanospheres that reduce exciton\u2010diffusion losses and enhance light harvesting and charge generation versus bulk COFs. Meanwhile, carboxylic acid groups incorporated into 1D nanopores tune the microenvironment to promote proton delivery. This unified design delivers an exceptional H\n 2<\/jats:sub>\n O\n 2<\/jats:sub>\n evolution rate of 11246\u00a0\u00b5mol g\n \u22121<\/jats:sup>\n \u00a0h\n \u22121<\/jats:sup>\n (>sevenfold enhancement over pristine bulk COF), and a solar\u2010to\u2010chemical conversion efficiency of 2.18% in pure water under air (AM 1.5G, 100\u00a0mW cm\n \u22122<\/jats:sup>\n ), among the highest reported for COF\u2010based photocatalysts. Experimental investigations and theoretical calculations reveal the carboxylated pore walls template continuous, oriented hydrogen\u2010bond chains in confined water, lowering the kinetic barrier for the 2e\n \u2212<\/jats:sup>\n ORR pathway. This work establishes a generalizable paradigm for orchestrating coupled proton\u2013electron transfer in porous photocatalysts for efficient solar energy conversion.\n <\/jats:p>","DOI":"10.1002\/anie.6474422","type":"journal-article","created":{"date-parts":[[2026,5,5]],"date-time":"2026-05-05T10:42:57Z","timestamp":1777977777000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":8,"title":["Synergizing Mass Transfer and Exciton Dissociation in Nanoscale COFs for Efficient H\n 2<\/sub>\n O\n 2<\/sub>\n Photosynthesis"],"prefix":"10.1002","volume":"65","author":[{"given":"Xinman","family":"Liu","sequence":"first","affiliation":[{"name":"State Key Laboratory of Green Chemical Engineering and Industrial Catalysis, Key Laboratory for Advanced Materials and Institute of Fine Chemicals, Shanghai Key Laboratory of Functional Materials Chemistry, Center of Photosensitive Chemicals Engineering, Feringa Nobel Prize Scientist Joint 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