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Herein, one\u2010dimensional porphyrin\u2010based covalent organic frameworks (designated as TD\u2010aniline and TD\u2010FeCl\n                    <jats:sub>3<\/jats:sub>\n                    ) with well\u2010defined structures were constructed under mild conditions via a novel synthesis strategy that employed aniline or FeCl\n                    <jats:sub>3<\/jats:sub>\n                    as crystallization modulators, thereby achieving efficient ROS generation and controllable activation of tumor cell pyroptosis. Notably, FeCl\n                    <jats:sub>3<\/jats:sub>\n                    not only promoted the ordered assembly of TD\u2010FeCl\n                    <jats:sub>3<\/jats:sub>\n                    but also introduced metal sites via coordination with porphyrin cores, resulting in superior sonodynamic performance compared to TD\u2010aniline. Specifically, metal coordination in TD\u2010FeCl\n                    <jats:sub>3<\/jats:sub>\n                    reduced its band gap to promote electron\u2010hole pair (e\n                    <jats:sup>\u2212<\/jats:sup>\n                    \u2013h\n                    <jats:sup>+<\/jats:sup>\n                    ) generation under ultrasound. Meanwhile, the introduced Fe\n                    <jats:sup>3+<\/jats:sup>\n                    diminished spatial e\n                    <jats:sup>\u2212<\/jats:sup>\n                    \u2013h\n                    <jats:sup>+<\/jats:sup>\n                    overlap in the excited state, thereby suppressing charge recombination, and ultimately channeling more excited\u2010state energy into a synergistic enhancement of superoxide anion and singlet oxygen production. Moreover, US irradiation enhanced the Fenton\u2010like activity of TD\u2010FeCl\n                    <jats:sub>3<\/jats:sub>\n                    . Based on its superior ROS generation capacity, TD\u2010FeCl\n                    <jats:sub>3<\/jats:sub>\n                    effectively promoted US\u2010triggered pyroptosis in tumor cells, leading to robust antitumor immune responses. This work establishes a novel paradigm for the controlled synthesis of one\u2010dimensional COFs and opens new avenues for pyroptosis\u2010based immunotherapy.\n                  <\/jats:p>","DOI":"10.1002\/anie.5056685","type":"journal-article","created":{"date-parts":[[2026,8,19]],"date-time":"2026-08-19T09:14:24Z","timestamp":1787130864000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Tailoring Crystallization Modulators for the Facile Synthesis of One\u2010Dimensional Covalent Organic Frameworks to Boost Ultrasound\u2010Triggered Pyroptosis and Immunotherapy"],"prefix":"10.1002","volume":"65","author":[{"given":"Jiwei","family":"Wang","sequence":"first","affiliation":[{"name":"Key Laboratory of Rare Earth Resource Utilization Changchun Institute of Applied Chemistry Chinese Academy of Sciences  Changchun Jilin China"},{"name":"School of Applied Chemistry and Engineering University of Science and Technology 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