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However, the synthesis of OIMHs has been largely confined to the use of pre\u2010synthesized, commercial organic cations, severely limiting structural diversity and functional exploration. Herein, we present a groundbreaking in situ synthetic paradigm that concurrently executes the Menshutkin reaction and crystal growth in a single step. This one\u2010pot strategy seamlessly couples the on\u2010site custom quaternization of organic precursors with the crystallization of metal halide frameworks (such as Mn\/Zn\/Sb halides). By decoupling the synthesis from commercial cation sources, this method provides unparalleled freedom to incorporate a vast array of tailored cations, including those with long\u2010chain, multi\u2010aryl, and sophisticated geometric motifs (e.g., boat, chair, wing, bowl, and cyclic architectures). The power of this approach is exemplified by a novel Mn\u2010based OIMH,\n                    <jats:bold>Py\u20102<\/jats:bold>\n                    ([B(3\u2010Br\u2010PyCH\n                    <jats:sub>2<\/jats:sub>\n                    )Ph]\n                    <jats:sub>3<\/jats:sub>\n                    [MnBr\n                    <jats:sub>4<\/jats:sub>\n                    ]\n                    <jats:sub>2<\/jats:sub>\n                    \u00b72Br), which acts as an exceptional X\u2010ray scintillator with a high light yield of 60,000 photons\/MeV\u20142.4 times that of commercial LuAG:Ce. A flexible scintillator screen fabricated from\n                    <jats:bold>Py\u20102<\/jats:bold>\n                    further demonstrates a high spatial resolution of 12.77 lp mm\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>1<\/jats:sup>\n                    , enabling high\u2010resolution X\u2010ray imaging. This work establishes a transformative in situ crystallization platform that opens a new dimension for the bespoke design of functional hybrid materials.\n                  <\/jats:p>","DOI":"10.1002\/anie.9721346","type":"journal-article","created":{"date-parts":[[2026,4,1]],"date-time":"2026-04-01T08:01:44Z","timestamp":1775030504000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":4,"title":["Unlocking Organic Cation Diversity in Metal Halides via Concurrent Crystal Growth and Menshutkin Reaction With Demonstrated Scintillation"],"prefix":"10.1002","volume":"65","author":[{"given":"Zhi","family":"Lin","sequence":"first","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Materials Science Fujian Normal University  Fuzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xue\u2010Fei","family":"He","sequence":"additional","affiliation":[{"name":"School of Physics and Optoelectronics South China University of Technology  Guangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guo\u2010Yang","family":"Chen","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou Fujian P.R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Bao\u2010Ling","family":"Tang","sequence":"additional","affiliation":[{"name":"School of Physics and Optoelectronics South China University of Technology  Guangzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ming\u2010Chang","family":"Wang","sequence":"additional","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Materials Science Fujian Normal University  Fuzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Rong\u2010Jie","family":"Xu","sequence":"additional","affiliation":[{"name":"The International Joint Institute of Tianjin University Fuzhou, Tianjin University  Tianjin China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jia\u2010Jia","family":"Li","sequence":"additional","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Materials Science Fujian Normal University  Fuzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jia\u2010Jie","family":"Liu","sequence":"additional","affiliation":[{"name":"Fujian Provincial Key Laboratory of Advanced Materials Oriented Chemical Engineering College of Chemistry and Materials Science Fujian Normal University  Fuzhou China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xiao\u2010Ying","family":"Huang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou Fujian P.R. 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