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Herein, we report a cobalt\u2010catalyzed allylic C\u2500H amidation of unactivated alkenes using dioxazolones as practical nitrene precursors. The isolation of a well\u2010defined \u03c0\u2010allyl\u2010cobalt(III) complex provides a platform for direct interrogation of the reactive nitrene species. Mechanistic studies, including EPR spectroscopy and DFT calculations, support the involvement of an open\u2010shell singlet cobalt\u2013nitrenoid intermediate. Both the neutral cobalt(III) precatalyst and the synthesized \u03c0\u2010allyl\u2010cobalt(III) complex are catalytically active, and the catalytic system displays broad substrate scope, good functional\u2010group tolerance, and moderate to high regioselectivity. These results provide key mechanistic insights into cobalt\u2010mediated nitrene transfer reactions and establish a foundation for the development of selective cobalt\u2010catalyzed C\u2500H amination reactions.<\/jats:p>","DOI":"10.1002\/anie.9432471","type":"journal-article","created":{"date-parts":[[2026,9,29]],"date-time":"2026-09-29T03:42:02Z","timestamp":1790653322000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Capturing an Elusive [Cp*Co(Allyl)CO]\n                    <sup>+<\/sup>\n                    Complex for Catalytic Allylic C\u2500H Amidation of Unactivated Olefins"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-6064-9317","authenticated-orcid":false,"given":"Rajib","family":"Mandal","sequence":"first","affiliation":[{"name":"Department of Chemistry Indian Institute of Technology Kanpur  Kanpur Uttar Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0003-7659-1337","authenticated-orcid":false,"given":"Abir","family":"Das","sequence":"additional","affiliation":[{"name":"Department of Chemistry Indian Institute of Technology Kanpur  Kanpur Uttar Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pritam","family":"Dolui","sequence":"additional","affiliation":[{"name":"Department of Chemistry Indian Institute of Technology Kanpur  Kanpur Uttar Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8232-5989","authenticated-orcid":false,"given":"Sayan","family":"Dutta","sequence":"additional","affiliation":[{"name":"Physical Science and Engineering Division King Abdullah University of Science and Technology (KAUST)  Thuwal Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-3818-1401","authenticated-orcid":false,"given":"Muralidharan","family":"Shanmugam","sequence":"additional","affiliation":[{"name":"Photon Science Institute and Department of Chemistry The University of Manchester  Manchester UK"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-5969-0112","authenticated-orcid":false,"given":"Bholanath","family":"Maity","sequence":"additional","affiliation":[{"name":"Physical Science and Engineering Division King Abdullah University of Science and Technology (KAUST)  Thuwal Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1398-338X","authenticated-orcid":false,"given":"Luigi","family":"Cavallo","sequence":"additional","affiliation":[{"name":"Physical Science and Engineering Division King Abdullah University of Science and Technology (KAUST)  Thuwal Saudi Arabia"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1112-137X","authenticated-orcid":false,"given":"Basker","family":"Sundararaju","sequence":"additional","affiliation":[{"name":"Department of Chemistry Indian Institute of Technology Kanpur  Kanpur Uttar Pradesh India"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,9,28]]},"reference":[{"key":"e_1_2_8_2_1","doi-asserted-by":"crossref","first-page":"347","DOI":"10.1007\/128_2009_19","volume-title":"C\u2500H Activation","author":"Zalatan D. 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