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In this work, we synthesize Ag\u2010decorated SnS\n                    <jats:sub>2<\/jats:sub>\n                    hollow microboxes using a coprecipitation method followed by a hydrothermal treatment. Based on a collection of in\u2010situ\/ex\u2010situ characterizations including in\u2010situ Raman spectroscopy, rapid freeze\u2010quench (RFQ)\n                    <jats:sup>119<\/jats:sup>\n                    Sn M\u00f6ssbauer spectroscopy, X\u2010ray diffraction (XRD), and X\u2010ray photoelectron spectroscopy (XPS), we discover that the Ag\u2010decorated SnS\n                    <jats:sub>2<\/jats:sub>\n                    (Ag@SnS\n                    <jats:sub>2<\/jats:sub>\n                    ) hollow microboxes undergo dynamic reduction and reconstruction during the electrochemical CO\n                    <jats:sub>2<\/jats:sub>\n                    RR, leading to the in\u2010situ formation of S\u2010doped Ag\u2013Sn alloy (S\u2010Ag\n                    <jats:sub>3<\/jats:sub>\n                    Sn\/Sn) hollow microboxes. This transformation results in a remarkable formate selectivity of 92.4% with a formate partial current density of 97.3 mA\u00b7cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    at \u22120.8\u00a0V versus RHE in an H\u2010cell. In\u2010situ attenuated total reflection surface\u2010enhanced infrared absorption spectroscopy (ATR\u2010SEIRAS) measurements and density functional theory (DFT) calculations indicate that both S\u2010doping and Ag\u2013Sn alloying enhance the CO\n                    <jats:sub>2<\/jats:sub>\n                    adsorption and improve the stability of *OCHO intermediate. This work offers a facile strategy for designing highly active and selective electrocatalyst for CO\n                    <jats:sub>2<\/jats:sub>\n                    RR.\n                  <\/jats:p>","DOI":"10.1002\/anie.202510743","type":"journal-article","created":{"date-parts":[[2025,6,30]],"date-time":"2025-06-30T22:00:03Z","timestamp":1751320803000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":24,"title":["S\u2010doped Ag\u2013Sn Alloy Hollow Microbox for High\u2010Performance CO\n                    <sub>2<\/sub>\n                    Electroreduction to Formate"],"prefix":"10.1002","volume":"64","author":[{"given":"Wenwen","family":"Zhang","sequence":"first","affiliation":[{"name":"School of Chemical Engineering Dalian University of Technology  Dalian 116024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qing","family":"Mao","sequence":"additional","affiliation":[{"name":"School of Chemical Engineering Dalian University of Technology  Dalian 116024 China"},{"name":"State Key Laboratory of Fine Chemistry Frontier Science Center for Smart Materials School of Chemical Engineering Dalian University of Technology  Dalian 116024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jie","family":"Ding","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering City University of Hong Kong  Hong Kong SAR 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qi","family":"Liu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Fine Chemistry Frontier Science Center for Smart Materials School of Chemical Engineering Dalian University of Technology  Dalian 116024 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Shifu","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Catalysis Dalian Institute of Chemical Physics Chinese Academy of Sciences  Dalian 116023 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiuyi","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Catalysis Dalian Institute of Chemical Physics Chinese Academy of Sciences  Dalian 116023 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xuning","family":"Li","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Catalysis Dalian Institute of Chemical Physics Chinese Academy of Sciences  Dalian 116023 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongbin","family":"Yang","sequence":"additional","affiliation":[{"name":"School of Materials Science and Engineering Suzhou University of Science and Technology  Suzhou 215011 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4685-2052","authenticated-orcid":false,"given":"Bin","family":"Liu","sequence":"additional","affiliation":[{"name":"Department of Materials Science and Engineering City University of Hong Kong  Hong Kong SAR 999077 China"},{"name":"Department of Chemistry Hong Kong Institute for Clean Energy (HKICE) &amp; Center of Super\u2010Diamond and Advanced Films (COSDAF) City University of Hong Kong  Hong Kong SAR 999077 China"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"311","published-online":{"date-parts":[[2025,7,24]]},"reference":[{"key":"e_1_2_8_1_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41560-017-0078-8"},{"key":"e_1_2_8_2_1","doi-asserted-by":"publisher","DOI":"10.1021\/acscatal.1c05272"},{"key":"e_1_2_8_3_1","doi-asserted-by":"publisher","DOI":"10.1002\/anie.202410932"},{"key":"e_1_2_8_4_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-019-08805-x"},{"key":"e_1_2_8_5_1","doi-asserted-by":"publisher","DOI":"10.1038\/s41467-021-26124-y"},{"key":"e_1_2_8_6_1","doi-asserted-by":"publisher","DOI":"10.1002\/aenm.202070046"},{"key":"e_1_2_8_7_1","volume":"62","author":"Zhao S.","year":"2019","journal-title":"Nano\u2010Micro Lett."},{"key":"e_1_2_8_8_1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.202005113"},{"key":"e_1_2_8_9_1","first-page":"117","volume":"36","author":"Jianjian T.","year":"2021","journal-title":"J Inorg. 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