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A sustainable synthesis route involves the green electrochemical coupling of CO\n                    <jats:sub>2<\/jats:sub>\n                    with dimethylamine (DMA). However, the rational design of highly efficient catalysts for this transformation remains constrained by a limited mechanistic understanding of the key reactive intermediates governing the process. In this study, *COO is identified as the pivotal intermediate facilitating C\u2500N coupling, a finding substantiated by in situ Fourier transform infrared spectroscopy (FT\u2010IR) and online differential mass spectrometry (DEMS). Complementary Raman spectroscopy analyses further revealed that the intermediate adopts a stable chair\u2010like configuration, characterized by dual\u2010coordinated adsorption through both C and O atoms. Based on these mechanistic insights, a ZnCu catalyst was engineered that facilitates efficient CO\n                    <jats:sub>2<\/jats:sub>\n                    activation while simultaneously stabilizing this adsorption configuration, thereby enhancing the C\u2500N coupling pathway. As a result, a DMF Faradaic efficiency (FE\n                    <jats:sub>DMF<\/jats:sub>\n                    ) of 51% and a production rate of 575\u00a0mmol\u00b7g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00b7h\n                    <jats:sup>\u22121<\/jats:sup>\n                    are achieved, outperforming all previously reported catalytic systems under comparable conditions. This study establishes a robust framework for understanding and optimizing C\u2500N coupling via precise intermediate stabilization.\n                  <\/jats:p>","DOI":"10.1002\/anie.4379815","type":"journal-article","created":{"date-parts":[[2026,6,23]],"date-time":"2026-06-23T08:03:59Z","timestamp":1782201839000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Regulating the Adsorption Configuration of Intermediates to Construct C\u2500N Bonds From CO\n                    <sub>2<\/sub>\n                    for High\u2010Efficiency\n                    <i>N<\/i>\n                    ,\n                    <i>N<\/i>\n                    \u2010Dimethylformamide Electrosynthesis"],"prefix":"10.1002","volume":"65","author":[{"given":"Yunhui","family":"Yan","sequence":"first","affiliation":[{"name":"State Key Laboratory of Chemo and Biosensing College of Chemistry and Chemical Engineering International Joint Lab of Energy Electrochemistry of the Ministry of Education Hunan University  Changsha P. 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