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Here, we present, for the first time, a novel strategy of constructing asymmetric \u201cintramolecular electron compartments\u201d (IEC) in single metal\u2013organic frameworks (MOFs) that enables efficient PCOR to multielectron products. The resulting Cu\u2010MOF\u2010NK1(BF\n                    <jats:sub>4<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    ) achieves a remarkable CH\n                    <jats:sub>3<\/jats:sub>\n                    OH production rate of 115.8\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    (92.0% selectivity) without using any sacrificial agents and cocatalysts, making it one of the top\u2010performing single\u2010component PCOR catalysts reported to date. Notably, under simulating flue gas condition (15% CO\n                    <jats:sub>2<\/jats:sub>\n                    ), it remains the remarkable performance of 110.2\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    with corresponding total electron assumption rate of 661.2\u00a0\u00b5mol g\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    , the highest value reported to date, setting a benchmark for low\u2010concentration CO\n                    <jats:sub>2<\/jats:sub>\n                    photocatalysts in overall reaction. Combined experimental and theoretical studies reveal new insights that the presence of asymmetric IEC within MOFs accounts for the enhanced accumulation of photogenerated electrons, thereby promoting the production of multielectron products. Our work not only develops a promising photocatalyst for converting CO\n                    <jats:sub>2<\/jats:sub>\n                    and H\n                    <jats:sub>2<\/jats:sub>\n                    O to methanol, but also establishes a universal design principle for constructing single\u2010component PCOR catalysts that enable multielectron reduction products.\n                  <\/jats:p>","DOI":"10.1002\/anie.202520298","type":"journal-article","created":{"date-parts":[[2025,12,23]],"date-time":"2025-12-23T12:08:51Z","timestamp":1766491731000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":9,"title":["Single MOF Based on Asymmetric Intramolecular Electron Compartments Enables Highly Efficient Photocatalytic CO\n                    <sub>2<\/sub>\n                    Overall Reaction to Methanol"],"prefix":"10.1002","volume":"65","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-6868-2472","authenticated-orcid":false,"given":"Qiao","family":"Zhao","sequence":"first","affiliation":[{"name":"School of Materials Science and Engineering, National Institute for Advanced Materials, TKL of Metal and Molecule\u2010Based Material Chemistry, State Key Laboratory of Elemento\u2010Organic Chemistry, Frontiers Science Center for New Organic Matter, College of Chemistry Academy for Advanced Interdisciplinary Studies, Nankai University  Tianjin P.R. 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