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Generally, the cross\u2010coupling selectivity is achieved by the persistent radical effect (PRE) that requires the presence of a persistent radical and a transient radical, thus resulting in limited radical precursors. In this paper, a highly selective cross\u2010coupling of alkyl radicals with acyl radicals to construct C(sp\n                    <jats:sup>2<\/jats:sup>\n                    )\u2212C(sp\n                    <jats:sup>3<\/jats:sup>\n                    ) bonds, or with alkyl radicals to construct C(sp\n                    <jats:sup>3<\/jats:sup>\n                    )\u2212C(sp\n                    <jats:sup>3<\/jats:sup>\n                    ) bonds have been achieved with the readily available carboxylic acids and their derivatives (NHPI ester) as coupling partners. The success originates from the use of tridentate ligand (2,2\u2032\u2009:\u20096\u2032,2\u2032\u2032\u2010terpyridine) to enable radical cross\u2010coupling process to Ni\u2010mediated organometallic mechanism. This protocol offers a facile and flexible access to structurally diverse ketones (up to 90\u2009% yield), and also a new solution for the challenging double decarboxylative C(sp\n                    <jats:sup>3<\/jats:sup>\n                    )\u2212C(sp\n                    <jats:sup>3<\/jats:sup>\n                    ) coupling. The broad utility and functional group tolerance are further illustrated by the late\u2010stage functionalization of natural\u2010occurring carboxylic acids and drugs.\n                  <\/jats:p>","DOI":"10.1002\/anie.202405866","type":"journal-article","created":{"date-parts":[[2024,5,24]],"date-time":"2024-05-24T13:14:53Z","timestamp":1716556493000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":56,"title":["Nickel\u2010Catalyzed Highly Selective Radical C\u2212C Coupling from Carboxylic Acids with Photoredox Catalysis"],"prefix":"10.1002","volume":"63","author":[{"given":"Bo","family":"Ling","sequence":"first","affiliation":[{"name":"State Key Laboratory of Coordination Chemistry Jiangsu Key Laboratory of Advanced Organic Materials Chemistry and Biomedicine Innovation Center (ChemBIC) School of Chemistry and Chemical Engineering Nanjing University  Nanjing 210023 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