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Herein, we report a Co\u2013Mn heteronuclear single\u2011atom catalyst (Co\n                    <jats:sub>1<\/jats:sub>\n                    \u2010Mn\n                    <jats:sub>1<\/jats:sub>\n                    \/NC) in which atomically dispersed Co and Mn species are anchored on a nitrogen\u2011doped carbon support to form well\u2011defined neighboring active pairs with an interatomic distance of \u223c2.6\u00a0\u00c5. This configuration provides a synergistic platform that markedly outperforms its monometallic Co and Mn counterparts in two challenging oxidative C\u2013H functionalization reactions: the selective oxidation of acenaphthene to 1\u2011acenaphthenol (99.9% conversion, 97.7% selectivity) and the oxidative condensation of benzyl alcohol with methanol to benzaldehyde dimethyl acetal (63.4% conversion, 94.7% selectivity). Atomic\u2011resolution characterization and DFT calculations elucidate the origin of this synergy, revealing a division of labor between the two metal centers. In acenaphthene oxidation, the Co\u2013Mn pair cooperatively activates molecular oxygen and facilitates C\u2013H bond dissociation with a substantially reduced energy barrier. In the oxidative condensation, the Co site preferentially activates methanol while the adjacent Mn site stabilizes the key *PhCHO intermediate. This work establishes heteronuclear neighboring Co\u2013Mn pairs as a platform for synergistic multifunctional catalysis.\n                  <\/jats:p>","DOI":"10.1002\/anie.2619409","type":"journal-article","created":{"date-parts":[[2026,5,27]],"date-time":"2026-05-27T07:16:01Z","timestamp":1779866161000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Heteronuclear Neighboring Co\u2013Mn Single\u2010Atom Pairs as a Synergistic Platform for Oxidative C\u2013H Functionalization"],"prefix":"10.1002","volume":"65","author":[{"given":"Wen","family":"Jiang","sequence":"first","affiliation":[{"name":"Key Laboratory of the Ministry of Education for Advanced Catalysis Materials Zhejiang Key Laboratory of Advanced Catalysis and Adsorption Materials Institute of Physical Chemistry Zhejiang Normal University  Jinhua People's Republic of 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