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Herein, we report an unprecedented copper\u2010catalyzed enantioselective C\u2013H phosphorylation through oxidative C\u2013H\/P\u2013H coupling. This method employs earth\u2010abundant copper catalyst and readily accessible 3,3\u2032\u2010difluorinated BINOL (1,1'\u2010bi\u20102\u2010naphthol) ligand, which proved essential for achieving high reactivity and enantioselectivity. A broad range of unmasked H\u2010phosphonates and secondary phosphine oxides (SPOs) serve as practical coupling partners, delivering planar\u2010chiral metallocenes in good yields with high enantioselectivity (up to 99:1 er). The robustness of this approach is demonstrated through gram\u2010scale synthesis, facile directing\u2010group removal, and versatile downstream transformations. Furthermore, the resulting chiral phosphines were applied as a new class of Lewis base catalysts in the enantioselective allylation of aldehydes, underscoring their potential utility in asymmetric synthesis.<\/jats:p>","DOI":"10.1002\/anie.8768278","type":"journal-article","created":{"date-parts":[[2026,5,21]],"date-time":"2026-05-21T12:44:34Z","timestamp":1779367474000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Copper\u2010Catalyzed Enantioselective C\u2013H Phosphorylation Enabled by a 3,3\u2019\u2010Difluorinated BINOL Ligand"],"prefix":"10.1002","volume":"65","author":[{"given":"Qiang","family":"Yue","sequence":"first","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lei","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hui\u2010Nan","family":"Ren","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhuo\u2010Zhuo","family":"Zhang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-7258-2845","authenticated-orcid":false,"given":"Tao","family":"Zhou","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-2872-7688","authenticated-orcid":false,"given":"Qi\u2010Jun","family":"Yao","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0375-955X","authenticated-orcid":false,"given":"Bing\u2010Feng","family":"Shi","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Soil Pollution Control and Safety Department of Chemistry Zhejiang University  Hangzhou China"},{"name":"College of Material Chemistry and Chemical Engineering Key Laboratory of Organosilicon Chemistry and Material Technology Ministry of Education Hangzhou Normal University  Hangzhou Zhejiang China"},{"name":"State Key Laboratory of Coordination Chemistry Nanjing University  Nanjing China"},{"name":"School of Chemistry and Chemical Engineering Henan Normal University  Henan China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2026,5,21]]},"reference":[{"key":"e_1_2_10_2_1","first-page":"3","volume-title":"Ferrocenes: Homogeneous Catalysis, Organic Synthesis, Materials Science","author":"Togni A.","year":"1995"},{"key":"e_1_2_10_3_1","first-page":"1","volume-title":"Chiral Ferrocenes in AsymmetricCatalysis","author":"Dai L. 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