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In particular, aerobic hydroxylation of allylic and propargylic C\u2500H bonds is difficult due to overoxidation and competing side reactions. Here we report a heterogeneous catalyst featuring atomically dispersed iron sites embedded in a nitrogen\u2010doped carbon matrix. This catalyst enables unprecedented site\u2010 and chemoselective allylic and propargylic C\u2500H hydroxylation of alkenes and alkynes using air as the oxidant at 30\u00b0C. The method accommodates a broad range of terminal and internal substrates with excellent functional\u2010group tolerance and enables late\u2010stage oxidation of structurally complex molecules. Mechanistic studies demonstrate that the catalytic activity originates from highly dispersed FeN\n                    <jats:sub>x<\/jats:sub>\n                    sites. This work highlights the potential of single\u2010atom catalysis to address fundamental challenges in sustainable C\u2500H oxidation and expands the toolbox for selective oxidative transformations.\n                  <\/jats:p>","DOI":"10.1002\/anie.2913960","type":"journal-article","created":{"date-parts":[[2026,6,11]],"date-time":"2026-06-11T05:59:16Z","timestamp":1781157556000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Atomically Dispersed Iron\u2010Catalyzed Aerobic Hydroxylation of Allylic and Propargylic C\u2500H Bonds"],"prefix":"10.1002","volume":"65","author":[{"given":"Yijie","family":"Jiang","sequence":"first","affiliation":[{"name":"Key Laboratory of Material Chemistry For Energy Conversion and Storage, Ministry of Education Hubei Key Laboratory of Material Chemistry and Service Failure School of Chemistry and Chemical Engineering Huazhong University of Science and Technology  Wuhan 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