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Dual\u2010atom catalysts have attracted considerable attention due to their unique cooperative effects. Herein, we report a porous organic polymer\u2010supported Rh\n                    <jats:sub>1<\/jats:sub>\n                    \u2013Cu\n                    <jats:sub>1<\/jats:sub>\n                    dual\u2010site catalyst (Rh\n                    <jats:sub>1<\/jats:sub>\n                    \u2013Cu\n                    <jats:sub>1<\/jats:sub>\n                    @POPs\u2010PPh\n                    <jats:sub>3<\/jats:sub>\n                    ) for the selective oxidation of ethane to ethanol, acetaldehyde, and acetic acid with auto\u2010selective oxygen mechanism. The optimized Rh\n                    <jats:sub>1<\/jats:sub>\n                    \u2013Cu\n                    <jats:sub>1<\/jats:sub>\n                    centers deliver a productivity of ca. 250\u00a0mol mol\n                    <jats:sub>Rh<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    h\n                    <jats:sup>\u22121<\/jats:sup>\n                    based on Rh with 65% acetaldehyde selectivity at 423 K, representing a four\u2010fold improvement over the single\u2010Rh\u2010site catalyst. Through isotopic labeling and in situ characterizations, we uncover an auto\u2010selective oxygen source mechanism in which dehydrogenated species of ethane with different grades possess self\u2010selectivity for the combined oxygen source. Oxygen species derived from O\n                    <jats:sub>2<\/jats:sub>\n                    activate ethane and subsequently couple with the ethyl fragment to produce ethanol. While OH radicals from H\n                    <jats:sub>2<\/jats:sub>\n                    O dissociation react with ethyl intermediates from ethane dehydrogenation to yield acetaldehyde. Concurrently, oxygen species recombine with reactive hydrogen species to regenerate new H\n                    <jats:sub>2<\/jats:sub>\n                    O, completing the catalytic oxidation cycle. The density functional theory (DFT) calculations reveal that the Rh\u2013Cl\u2013Cu configuration lowers the lowest unoccupied molecular orbital (LUMO) energy of Rh\n                    <jats:sub>1<\/jats:sub>\n                    , thereby strengthening adsorbate\u2010metal interactions, weakening the C\u2500H bond, and facilitating its activation.\n                  <\/jats:p>","DOI":"10.1002\/anie.202521562","type":"journal-article","created":{"date-parts":[[2026,2,4]],"date-time":"2026-02-04T06:36:57Z","timestamp":1770187017000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Synergistic Rh\n                    <sub>1<\/sub>\n                    \u2013Cu\n                    <sub>1<\/sub>\n                    Dual\u2010Atom\u2010Site Enhancing Performance of Ethane Low\u2010Temperature Oxidation via Auto\u2010Selective Oxygen Source From O\n                    <sub>2<\/sub>\n                    \/H\n                    <sub>2<\/sub>\n                    O"],"prefix":"10.1002","volume":"65","author":[{"given":"Bin","family":"Li","sequence":"first","affiliation":[{"name":"Dalian National Laboratory for Clean Energy Dalian Institute of Chemical Physics Chinese Academy of Sciences  Dalian China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Siquan","family":"Feng","sequence":"additional","affiliation":[{"name":"Dalian National Laboratory for Clean Energy Dalian Institute of Chemical Physics Chinese Academy of Sciences  Dalian China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiaqian","family":"Wang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiangen","family":"Song","sequence":"additional","affiliation":[{"name":"Dalian National Laboratory for Clean Energy Dalian Institute of Chemical Physics Chinese Academy of 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