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While pathway selection is typically interpreted in terms of molecular packing, the potential regulatory role of organization beyond the molecular scale remains largely unexplored. Here we demonstrate that hierarchical mesoscale aggregation can control pathway selection during supramolecular polymerization. A donor\u2013acceptor dicyanostilbene derivative forms two primary aggregates that further assemble into mesoscale structures under concentrated conditions. Time\u2010resolved small\u2010angle x\u2010ray scattering combined with spectroscopy reveals that mesoscale clusters transiently trap metastable assemblies, thereby delaying their conversion into thermodynamically favored fibers. Increasing temperature enables escape from this mesoscale trap, directly switching the assembly pathway. These findings identify mesoscale trapping as an emergent kinetic regulatory mechanism in supramolecular polymerization.<\/jats:p>","DOI":"10.1002\/anie.7258562","type":"journal-article","created":{"date-parts":[[2026,5,9]],"date-time":"2026-05-09T16:01:53Z","timestamp":1778342513000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Hierarchical Mesoscale Trapping Controls Pathway Selection in Supramolecular Polymerization"],"prefix":"10.1002","volume":"65","author":[{"given":"Ziyuan","family":"Li","sequence":"first","affiliation":[{"name":"School of Nuclear Science and Technology University of Science and Technology of China  Hefei Anhui P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Rongzhou","family":"Du","sequence":"additional","affiliation":[{"name":"National Synchrotron Radiation Laboratory University of Science and Technology of China  Hefei Anhui P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yun","family":"Huang","sequence":"additional","affiliation":[{"name":"School of Nuclear Science and Technology University of Science and Technology of China  Hefei Anhui P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6452-4370","authenticated-orcid":false,"given":"Ningdong","family":"Huang","sequence":"additional","affiliation":[{"name":"School of Nuclear Science and Technology University of Science and Technology of China  Hefei Anhui P. R. China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3826-5579","authenticated-orcid":false,"given":"Feng","family":"Wang","sequence":"additional","affiliation":[{"name":"Department of Polymer Science and Engineering State Key Laboratory of Precision and Intelligent Chemistry University of Science and Technology of China  Hefei Anhui P. R. 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