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In this work, we achieve the first surface\u2010confined synthesis of monolayer COF via Wurtz coupling, demonstrating prominent stereoselectivity through temperature modulation. At reduced temperature (78 K), the reaction preferentially follows a\n                    <jats:italic>trans<\/jats:italic>\n                    \u2010coupling pathway, enabling the successful synthesis of metastable COF that maintains structural integrity during thermal treatment due to surface confinement. Conversely, deposition at elevated temperature (298 K) promotes thermodynamically stable\n                    <jats:italic>cis<\/jats:italic>\n                    \u2010coupling porous nanoribbons. Combined ultrahigh\u2010vacuum scanning tunneling microscopy (UHV\u2010STM) and density functional theory (DFT) calculations elucidate the fundamental thermodynamic\u2010kinetic competition mechanism governing the C\u2010C coupling reactions at the molecular level: while the\n                    <jats:italic>trans<\/jats:italic>\n                    \u2010coupling pathway benefits from a lower activation barrier, the\n                    <jats:italic>cis<\/jats:italic>\n                    \u2010coupling configuration represents the thermodynamic minimum. Notably, this synthetic approach demonstrates pronounced generality, as confirmed by its successful implementation with another triphenylbenzyl bromide precursor to yield monolayer COF. This work deepens the understanding of irreversible bond formation in on\u2010surface synthesis and establishes kinetic trapping as a powerful strategy for achieving precise stereoselective control in Wurtz coupling.\n                  <\/jats:p>","DOI":"10.1002\/anie.5815461","type":"journal-article","created":{"date-parts":[[2026,2,5]],"date-time":"2026-02-05T05:28:17Z","timestamp":1770269297000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":3,"title":["Surface\u2010Assisted Wurtz Coupling for the Stereoselective Synthesis of Covalent Organic Frameworks"],"prefix":"10.1002","volume":"65","author":[{"given":"Minjie","family":"Xu","sequence":"first","affiliation":[{"name":"Key Laboratory of Polyoxometalate and Reticular Material Chemistry of Ministry of Education Northeast Normal University  Changchun P. R. 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