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However, challenges such as the high cost and limited sustainability of Ir complexes hinder its broader application. In this study, we designed three metal\u2013organic layers (MOLs) and immobilized functionalized Ir photosensitizers (Ir\u2010PSs) on their surfaces via coordination exchange or click chemistry, yielding six MOL\u2013PSs hybrids. Chiral Ni complexes also adhere to the MOL surface through coordination bonds. These dual catalysts exhibited enantioselectivity (up to 99%\u00a0ee) superior to that of Ir\u2010PF\n                    <jats:sub>6<\/jats:sub>\n                    in the asymmetric acylation of saturated\n                    <jats:italic>N<\/jats:italic>\n                    \u2010heterocycles at \u03b1\u2010C(sp\n                    <jats:sup>3<\/jats:sup>\n                    )\u2500H bonds. The enhanced enantioselectivity of the MOL\u2013PSs over Ir\u2010PF\n                    <jats:sub>6<\/jats:sub>\n                    likely arises from steric change of chiral Ni complexes coordinating with hydroxyl or amine groups on the MOLs, which also form ion pairs with Ir\u2010PSs. This strategy demonstrates broad applicability across diverse chiral ligands and substrates, underscoring the potential of using MOLs in asymmetric photocatalysis to enhance both enantioselectivity and catalyst reusability.\n                  <\/jats:p>","DOI":"10.1002\/anie.202518424","type":"journal-article","created":{"date-parts":[[2025,10,17]],"date-time":"2025-10-17T11:07:27Z","timestamp":1760699247000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":14,"title":["Iridium Photosensitizers Immobilized on Metal\u2013Organic Layers Lead to Enhanced Enantioselectivity in Ni\/Ir Dual Photocatalysis"],"prefix":"10.1002","volume":"64","author":[{"given":"Yuanzhao","family":"Peng","sequence":"first","affiliation":[{"name":"iChem State Key Laboratory of Physical Chemistry of Solid Surfaces College of Chemistry and Chemical Engineering Xiamen University  422 South Siming Rd., Siming District Xiamen Fujian 361005 P.R. 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