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Herein, we report a self\u2010sustained biosolar reaction platform that integrates binary alkali\u2010metal\u2010doped carbon nitride (ACN) with a cytochrome P450 enzyme (peroxygenase CYP152A1). The sodium\u2010potassium co\u2010doped ACN (NaK\u2010ACN) photocatalyst exhibits an enhanced surface built\u2010in electric field, arising from the synergistic effects of the alkali metal dopants, enabling an efficient two\u2010electron oxygen reduction reaction (2e\n                    <jats:sup>\u2212<\/jats:sup>\n                    ORR) under visible\u2010light irradiation. Concurrently, CYP152A1 rapidly consumes the in situ generated H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    to catalyze the regioselective hydroxylation of tetradecanoic acid (C\n                    <jats:sub>14<\/jats:sub>\n                    ). This light\u2010driven cascade achieved \u03b1\u2010 and \u03b2\u2010hydroxylation activities 37.8 and 39.2 fold higher than those of conventional systems relying on an exogenous H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    supply. Collectively, this study establishes a biosolar cascade that couples the photocatalytic oxygen reduction reaction with regioselective enzymatic oxyfunctionalization, providing a versatile platform for solar\u2010driven oxidation of aliphatic substrates.\n                  <\/jats:p>","DOI":"10.1002\/smll.75979","type":"journal-article","created":{"date-parts":[[2026,9,27]],"date-time":"2026-09-27T16:42:46Z","timestamp":1790527366000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Regioselective C\u2010H Oxyfunctionalization of Aliphatic Acids Through a Consecutive Biosolar Cascade"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-0365-6529","authenticated-orcid":false,"given":"Chung Hyun","family":"Lee","sequence":"first","affiliation":[{"name":"Department of Materials Science and Engineering Korea Advanced Institute of Science and Technology (KAIST)  Daejeon Republic of 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