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We report herein mechanochemical (MC) nucleophilic aromatic substitution (S\n                    <jats:sub>N<\/jats:sub>\n                    Ar) that enables sulfur conversion into thianthrene\u2010bridged porous ladder polymer networks with dense donor\u2010acceptor (D\u2212A) molecular junctions. We demonstrate that the key lies in the generation of bent thianthrene units through a solid\u2010state ball\u2010milling condensation reaction between 1,2\u2010dihaloarenes and elemental sulfur. We also show that the assembling of D\u2212A structural motifs into porous networks affords efficient visible\u2010light\u2010driven photocatalytic reduction of carbon dioxide (CO\n                    <jats:sub>2<\/jats:sub>\n                    ) with water (H\n                    <jats:sub>2<\/jats:sub>\n                    O) vapor, in the absence of any additional photosensitizer, sacrificial agents or cocatalysts. Exceptional photoinduced charge separation along with boosted exciton dissociation results in a high\u2010performance of carbon monoxide (CO) production rate of 306.1\u2005\u03bcmol\u2009g\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u2009h\n                    <jats:sup>\u22121<\/jats:sup>\n                    with near 100\u2009% CO selectivity, which is accompanied by H\n                    <jats:sub>2<\/jats:sub>\n                    O oxidation to O\n                    <jats:sub>2<\/jats:sub>\n                    , as confirmed by both experimental and theoretical results. We anticipate this novel MC S\n                    <jats:sub>N<\/jats:sub>\n                    Ar approach will advance processing techniques for direct sulfur utilization and facilitate new possibilities for the synthesis of D\u2212A ladder polymer networks with promising potential in photocatalysis.\n                  <\/jats:p>","DOI":"10.1002\/anie.202419108","type":"journal-article","created":{"date-parts":[[2025,2,11]],"date-time":"2025-02-11T02:38:22Z","timestamp":1739241502000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Sulfur Conversion to Donor\u2010Acceptor Ladder Polymer Networks through Mechanochemical Nucleophilic Aromatic Substitution for Efficient CO\n                    <sub>2<\/sub>\n                    Photoreduction"],"prefix":"10.1002","volume":"64","author":[{"given":"Na","family":"Yang","sequence":"first","affiliation":[{"name":"School of Carbon Neutrality Future Technology Sichuan University  Chengdu 610065 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zi\u2010Jian","family":"Zhou","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Green Chemical Engineering and Industrial Catalysis Centre for Computational Chemistry and Research Institute of Industrial Catalysis School of Chemistry and Molecular Engineering East China University of Science and Technology  Shanghai 200237 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3973-4998","authenticated-orcid":false,"given":"Xiang","family":"Zhu","sequence":"additional","affiliation":[{"name":"School of Carbon Neutrality Future Technology Sichuan University  Chengdu 610065 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiwei","family":"Wu","sequence":"additional","affiliation":[{"name":"School of Carbon Neutrality Future Technology Sichuan University  Chengdu 610065 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