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Hydroboration of alkenes with hydroboranes is a reliable route to access organoboron compoundsssssss, yet the Markovnikov\u2010selective hydroboration of unactivated terminal alkenes remains challenging. In this study, we report a triple catalysis strategy for the highly Markovnikov\u2010selective hydroboration of unactivated terminal alkenes with HBaza\u2010type hydroborane (HBaza: 1,3,2\u2010benzodiazaborolane). The reaction exhibits a broad substrate scope and good functional group compatibility, and has been successfully applied to the Markovnikov hydroboration of alkene derivatives from complex molecules. Further derivatizations of the resulting alkyl boron products, as well as the synthesis of biologically relevant molecules or intermediates, highlight the synthetic value of this method. Mechanistic studies support that this reaction proceeds via sequential metal\u2010hydride hydrogen atom transfer (MHAT)\u2010mediated radical generation and HBaza\u2010involved radical borylation process under a triple photoredox, cobalt, and Br\u00f8nsted acid catalysis.<\/jats:p>","DOI":"10.1002\/anie.5679433","type":"journal-article","created":{"date-parts":[[2026,10,4]],"date-time":"2026-10-04T10:12:53Z","timestamp":1791108773000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Radical Markovnikov Hydroboration of Unactivated Terminal Alkenes With HBaza\u2010Type Hydroborane via a Triple Catalysis"],"prefix":"10.1002","author":[{"given":"Chang","family":"Liu","sequence":"first","affiliation":[{"name":"Key Laboratory of Molecule Synthesis and Function Discovery Fujian Province University College of Chemistry State Key Laboratory of Green and Efficient Development of Phosphorus Resources Fuzhou University  Fuzhou 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