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Here, a facile and scalable molecules\u2010confined pyrolysis approach is demonstrated for the synthesis of nitrogen\u2010coordinated transition\u2010metal (TM) single\u2010atom catalysts (SACs). Moreover, the various coordination structures of metal centers and the forms of nitrogen species are successfully revealed. The designed TM SACs show excellent catalytic performance for the cycloaddition of CO\n                    <jats:sub>2<\/jats:sub>\n                    with epoxides to cyclic carbonates under solvent\u2010free mild conditions. Among them, the optimum Zn SAC with 13.2\u00a0wt.% Zn content achieves a &gt;99% yield at 80\u00a0\u00b0C within 2\u00a0h for the cycloaddition of propylene oxide to propylene carbonate. The crucial comprehension of the relationship between performance and reaction mechanism over TM SACs with various metal centers and adjacent N species is further enhanced through experimental investigations and theoretical simulations.\u00a0Significantly, the high density of Lewis acid\u2013base sites (Zn and N species) can appropriately regulate the activation of epoxide and CO\n                    <jats:sub>2<\/jats:sub>\n                    and the reaction energy of cycloaddition, respectively, thus improving the CO\n                    <jats:sub>2<\/jats:sub>\n                    cycloaddition performance. This work provides a new insight into the design of highly active and stable SACs for efficient\u00a0cycloaddition reactions.\n                  <\/jats:p>","DOI":"10.1002\/smll.202500594","type":"journal-article","created":{"date-parts":[[2025,2,16]],"date-time":"2025-02-16T11:17:36Z","timestamp":1739704656000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":29,"title":["Engineering Nitrogen\u2010Coordinated Single\u2010Atom Catalysts for Efficient CO\n                    <sub>2<\/sub>\n                    Cycloaddition"],"prefix":"10.1002","volume":"21","author":[{"given":"Jiayi","family":"Li","sequence":"first","affiliation":[{"name":"School of Nuclear Science and Technology National Synchrotron Radiation Laboratory Key Laboratory of Precision and Intelligent Chemistry School of Chemistry and Materials Science Hefei National Research Center for Physical Sciences at the Microscale University of Science and Technology of China  Hefei Anhui 230026 P. 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