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However, overcoming the inherent incompatibility between metal and enzyme catalysts and optimizing their stability and activity to achieve effective synergy, remains a significant challenge. Here, we present an enzyme\u2010assisted, confined synthesis of metal nanoparticles (MNPs) within the nanochannels of covalent organic frameworks (COFs), to construct efficient enzyme\u2010metal hybrid catalysts for cascade reactions. The COF nanochannels stabilize the enzyme during MNP formation and the catalytic process, and synergize with the enzyme to regulate the size, dispersion, and electronic state of the MNPs through surface amino acid residues, realizing the co\u2010encapsulation and dual\u2010optimization of both components. Using Candida antarctica lipase B (CALB) and Pd nanoparticles as a model system, Pd\/CALB@COF exhibits an 8.2\u2010fold higher yield in the kinetic resolution (KR) of racemic 1\u2010phenylethylamine (1\u2010PEA), and a 2.7\u2010fold enhancement in racemization conversion, compared to counterparts without COF. Their synergy in dynamic kinetic resolution (DKR) delivers 91% yield, &gt;98% enantiomeric excess (e.e.) value, and recyclability, with applicability to various chiral amines. This strategy has been validated across different metal\u2010enzyme systems, establishing a versatile platform for designing efficient enzyme\u2010metal cascade systems.<\/jats:p>","DOI":"10.1002\/anie.202509105","type":"journal-article","created":{"date-parts":[[2025,7,8]],"date-time":"2025-07-08T10:35:34Z","timestamp":1751970934000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":18,"title":["Enzyme\u2010Assisted Confined Synthesis of Metal Nanoparticles in Covalent Organic Frameworks for Efficient Enzyme\u2010Metal Cascade Catalysis"],"prefix":"10.1002","volume":"64","author":[{"given":"Qin","family":"Wang","sequence":"first","affiliation":[{"name":"Beijing Key Laboratory of Photoelectronic\/Electrophotonic Conversion Materials Key Laboratory of Cluster Science Ministry of Education, Advanced Technology Research Institute (Jinan), Frontiers Science Center for High Energy Material, School of Interdisciplinary Science, School 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