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Herein, we design a two\u2010dimensional metal\u2013organic polymer catalyst featuring spatially adjacent Cu and 1H\u2010benzotriazole to form Cu\u2010\u03c0 units, which achieves a Faradaic efficiency of 61% for CH\n                    <jats:sub>4<\/jats:sub>\n                    at 800 mA\u00b7cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    . Using Infrared free\u2010electron laser (IRFEL) nanospectroscopy, we identify the key Cu\u2010\u03c0 coordination environment and low\u2010frequency bonding modes, unavailable by conventional IR techniques. Complementary in\u2010situ synchrotron radiation IR, electrochemical experiments and theoretical calculations reveal that \u03c0 sites adsorb hydrated cations, enabling localized hydrogen supply to adjacent *CO on Cu sites and suppressing long\u2010range hydrogen transfer\u2010induced side reactions. This inorganic\u2013organic synergy paves a new pathway to spatially match *H and *CO, advancing efficient CO\n                    <jats:sub>2<\/jats:sub>\n                    \u2010to\u2010hydrocarbons conversion.\n                  <\/jats:p>","DOI":"10.1002\/anie.4689245","type":"journal-article","created":{"date-parts":[[2026,5,18]],"date-time":"2026-05-18T12:01:51Z","timestamp":1779105711000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Metal\u2010\u03c0 Sites Localized Hydrogen\u2010*CO Coupling for Enhanced CO\n                    <sub>2<\/sub>\n                    Electromethanation"],"prefix":"10.1002","volume":"65","author":[{"given":"Mengyuan","family":"Liu","sequence":"first","affiliation":[{"name":"School of Nuclear Science and Technology Key Laboratory of Precision and Intelligent Chemistry Hefei National Research Center for Physical Sciences at the Microscale National Synchrotron Radiation Laboratory University of Science and Technology of China Hefei P.R. 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