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Herein, inspired by near\u2010infrared (NIR)\u2010activated multiphoton photocatalysis, a novel zinc\u2010based metal\u2010organic framework (ZnTBH) is reported, for the first time, to enable effective NIR\u2010mediated synergistic therapy through combined CO gas therapy and photodynamic therapy (PDT) in deep\u2010seated tumors. The engineered MOF integrates a V\u2010shaped Tr\u00f6ger's base (TB) derivative with an A\u2010\u03c0\u2010A configuration as the organic linker, synergistically enhancing CO\n                    <jats:sub>2<\/jats:sub>\n                    adsorption to overcome the \u201cdilute CO\n                    <jats:sub>2<\/jats:sub>\n                    \u201d challenge in tumors while enabling efficient endogenous CO\n                    <jats:sub>2<\/jats:sub>\n                    \u2010to\u2010CO conversion via NIR\u2010driven multiphoton photocatalysis. Moreover, the photogenerated holes localize on biphenyl\u20104,4'\u2010dicarboxylic acid can drive water oxidation to hydroxyl radicals (\u2022OH), thereby further improving therapeutic efficacy. This study presents a significant advancement in the design of NIR light\u2010driven photocatalytic systems for safe, precise, and localized CO delivery, offering new opportunities for CO\u2010based or combination therapies in the treatment of deep\u2010seated tumors.\n                  <\/jats:p>","DOI":"10.1002\/anie.202524756","type":"journal-article","created":{"date-parts":[[2026,1,27]],"date-time":"2026-01-27T13:22:35Z","timestamp":1769520155000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Near\u2010Infrared\u2010Activated Multiphoton Photocatalytic System for Synergistic Therapy via CO Generation and \u2022OH Production"],"prefix":"10.1002","volume":"65","author":[{"given":"Bo","family":"Li","sequence":"first","affiliation":[{"name":"Institutes of Physical Science and Information Technology School of Chemistry and Chemical Engineering Key Laboratory of Structure and Functional Regulation of Hybrid Materials Ministry of Education Anhui University  Hefei P.R. 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