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In contrast to the widely reported donor\u2010acceptor\u2010donor (D\u2010A\u2010D) type PSs, D\u2010A\u2010A\u2010D typed PSs are seldomly developed for the time\u2010consuming and complicated synthesis, but show great potential in enhancing ROS generation in phototheranostics. This work here presents a one\u2010step synthetic procedure of D\u2010A\u2010A\u2010D type 2DMeTPA\u20102BT with a high yield of 47%, which is significantly different from the previously reported dual\u2010acceptor cases. In contrast to 2DMeTPA\u2010BT, the dual\u2010acceptor PSs of 2DMeTPA\u20102BT display a much smaller \u0394<jats:italic>E<\/jats:italic><jats:sub>ST<\/jats:sub> value but large SOC constants. Also, the intersystem crossing (ISC) dynamics indicate that fast <jats:italic>k<\/jats:italic><jats:sub>ISC<\/jats:sub>, long \u03c4<jats:sub>Triplet<\/jats:sub>, and large triplet population are observed in 2DMeTPA\u20102BT\u2010based nanoparticles (NPs), contributing to a superior generation of ROS. 2DMeTPA\u20102BT NPs are then finally utilized for the imaging\u2010guided PDT <jats:italic>in vivo<\/jats:italic> with a tumor inhibition rate of 90%. This method offers an efficient way to produce dual\u2010acceptor typed PSs <jats:italic>via<\/jats:italic> a one\u2010step reaction, providing new avenues in high\u2010performance phototheranostics.<\/jats:p>","DOI":"10.1002\/smll.202411643","type":"journal-article","created":{"date-parts":[[2025,3,24]],"date-time":"2025-03-24T06:36:10Z","timestamp":1742798170000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":12,"title":["Turning Lemons into Lemonade: One\u2010Step Synthesized Dual\u2010Acceptor Organic Photosensitizer to Boost the Photodynamic Therapy"],"prefix":"10.1002","volume":"21","author":[{"given":"Zhi","family":"Wang","sequence":"first","affiliation":[{"name":"School of Chemistry Engineering Research Center of Energy Storage Materials and Devices Ministry of Education Xi'an Key Laboratory of Sustainable Polymer Materials Xi'an Jiao Tong University  Xi'an 710049 P. R. 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Youming","family":"Zhang","sequence":"additional","affiliation":[{"name":"Information Technology Research Institute Shenzhen Institute of Information Technology  Shenzhen 518172 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xuwei","family":"Luo","sequence":"additional","affiliation":[{"name":"School of Chemistry Engineering Research Center of Energy Storage Materials and Devices Ministry of Education Xi'an Key Laboratory of Sustainable Polymer Materials Xi'an Jiao Tong University  Xi'an 710049 P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yanzi","family":"Xu","sequence":"additional","affiliation":[{"name":"School of Chemistry Engineering Research Center of Energy Storage Materials and Devices Ministry of Education Xi'an Key Laboratory of Sustainable Polymer Materials Xi'an Jiao Tong University  Xi'an 710049 P. R. 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