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Cu\u2010based catalysts, as the most promising catalysts for high value\u2010added product generation, were often limited by slow CO generation and weak CO adsorption in practical applications. Guided by theoretical screening, herein, an atomic\u2010scale CuZn alloy cluster configuration was manipulated on covalent organic frameworks (COFs), and its CO\n                    <jats:sub>2<\/jats:sub>\n                    RR performance was further improved by the regulation of the electron\u2010donor functional groups. Through systematic characterization and theoretical simulations, we for the first time demonstrate and quantify the interstitial electrons in CuZn alloy clusters under the regulation of electron\u2010giving groups. Further in situ surface\u2010enhanced Raman spectroscopy (SERS) and simulation results reveal that the behavior of interstitial electrons with low work function and high mobility occupy the high\u2010energy orbital of the metal and easily transfer to *CO, therefore, the *CO is hydrogenated to *COH before coupling, and then the coupling energy barrier and path are optimized. Due to these attributes, the as\u2010developed CuZn alloy\u2010functionalized COF catalyst (CuZn\u2013COF\u2013OH) exhibits significantly improved activity and selectivity, with &gt;200\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    industrial\u2010grade current density and ethylene Faraday efficiency of up to \u223c79% at\u00a0\u22121.0\u00a0V versus RHE. This study provides innovative avenues and insights for the design and development of application\u2010oriented atomic\u2010scale catalysts.\n                  <\/jats:p>","DOI":"10.1002\/anie.202517420","type":"journal-article","created":{"date-parts":[[2025,11,21]],"date-time":"2025-11-21T06:59:42Z","timestamp":1763708382000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":6,"title":["Insight into the Behavior of Interstitial Electrons in CuZn Alloy\u2010Functionalized Covalent Organic Framework Catalysts for Enhanced CO\n                    <sub>2<\/sub>\n                    Electroreduction"],"prefix":"10.1002","volume":"65","author":[{"given":"Haizhong","family":"Zhang","sequence":"first","affiliation":[{"name":"Zhejiang Key Laboratory of Low\u2010carbon Control Technology for Industrial Pollution College of Environment Zhejiang University of Technology  No. 18 Chaowang Road Hangzhou 310014 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chao","family":"Zhu","sequence":"additional","affiliation":[{"name":"Zhejiang Key Laboratory of Low\u2010carbon Control Technology for Industrial Pollution College of Environment Zhejiang University of Technology  No. 18 Chaowang Road Hangzhou 310014 China"},{"name":"State Key Laboratory of Green Chemical Synthesis and Conversion Zhejiang University of Technology  Hangzhou 310014 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Renlan","family":"Liu","sequence":"additional","affiliation":[{"name":"College of Life and Environmental Science, Chashan University Town Wenzhou University  Wenzhou 325035 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jun","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Separation Membranes and Membrane Processes School of Environmental Science and Engineering Tiangong University  No. 399 Binshui West Road Tianjin 300387 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhen","family":"Qiu","sequence":"additional","affiliation":[{"name":"Ecological\u2010Environment &amp; Health College (EEHC) Zhejiang A &amp; F University  No.666 Wusu Street Hangzhou 310014 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qile","family":"Fang","sequence":"additional","affiliation":[{"name":"Advanced Institute of Natural Sciences Beijing Normal University  No. 18 Jinfeng Road Zhuhai 519087 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Weiting","family":"Yu","sequence":"additional","affiliation":[{"name":"Zhejiang Key Laboratory of Low\u2010carbon Control Technology for Industrial Pollution College of Environment Zhejiang University of Technology  No. 18 Chaowang Road Hangzhou 310014 China"},{"name":"State Key Laboratory of Green Chemical Synthesis and Conversion Zhejiang University of Technology  Hangzhou 310014 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shuang","family":"Song","sequence":"additional","affiliation":[{"name":"Zhejiang Key Laboratory of Low\u2010carbon Control Technology for Industrial Pollution College of Environment Zhejiang University of Technology  No. 18 Chaowang Road Hangzhou 310014 China"},{"name":"State Key Laboratory of Green Chemical Synthesis and Conversion Zhejiang University of Technology  Hangzhou 310014 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8977-7569","authenticated-orcid":false,"given":"Yi","family":"Shen","sequence":"additional","affiliation":[{"name":"Zhejiang Key Laboratory of Low\u2010carbon Control Technology for Industrial Pollution College of Environment Zhejiang University of Technology  No. 18 Chaowang Road Hangzhou 310014 China"},{"name":"State Key Laboratory of Green Chemical Synthesis and Conversion Zhejiang University of Technology  Hangzhou 310014 China"},{"name":"Shaoxing Research Institute Zhejiang University of Technology  Yangjing Lake Science and Technology Innovation Park Shaoxing 312000 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,11,20]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202107156"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41586\u2010019\u20101760\u20108"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41560\u2010019\u20100450\u2010y"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.2c00960"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1039\/C8CS00829A"},{"key":"e_1_2_8_6_1","doi-asserted-by":"publisher","DOI":"10.1021\/jacs.0c11450"},{"key":"e_1_2_8_7_1","doi-asserted-by":"publisher","DOI":"10.1002\/aenm.202100044"},{"key":"e_1_2_8_8_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202102320"},{"key":"e_1_2_8_9_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.201504766"},{"key":"e_1_2_8_10_1","first-page":"9735","volume":"142","author":"Zhao Y.","year":"2020","journal-title":"J. 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