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Herein, we report a methanol\u2010water mediated dual assembly pathway strategy for simultaneous construction of P and M helices in one\u2010component chiral system. The conformation of <jats:sc>l<\/jats:sc>\u2010phenylaniline derivates (LBpyF) is controlled to folded state in CH<jats:sub>3<\/jats:sub>OH due to the hydrogen bonds as well as C\u2212H\u22c5\u22c5\u22c5\u03c0 interaction between LBpyF and CH<jats:sub>3<\/jats:sub>OH. Addition of H<jats:sub>2<\/jats:sub>O into above CH<jats:sub>3<\/jats:sub>OH solution of LBpyF results in the simultaneous occurrence of two self\u2010assembly pathways and double networks of P and M helices were therefore formed, due to the synchronous process of 1)\u2005self\u2010assembly of folded LBpyF into M\u2010helices and 2)\u2005H<jats:sub>2<\/jats:sub>O induced unfolding of folded LBpyF molecules followed by self\u2010assembly of them into P\u2010helices. The bipyridine core, phenyl ring, amide unit all adapted into different stacking modes in M\u2010helices and P\u2010helices, and energy analysis indicated that the minority M\u2010helices were more thermodynamically favored products. This study provides an approach to explore synergetic evolution of multiple chiral structures by manipulating the multiple assembly pathway.<\/jats:p>","DOI":"10.1002\/anie.202417876","type":"journal-article","created":{"date-parts":[[2024,11,19]],"date-time":"2024-11-19T09:02:24Z","timestamp":1732006944000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":11,"title":["Simultaneous Fabrication of P and M Helices in One\u2010Component Chiral System by Methanol\u2010Water Mediated Dual Assembly Pathway"],"prefix":"10.1002","volume":"64","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-0335-4675","authenticated-orcid":false,"given":"Laiben","family":"Gao","sequence":"first","affiliation":[{"name":"State Key Lab of Metal Matrix Composites School of Materials Science and Engineering Shanghai Key Laboratory for Molecular Engineering of Chiral Drugs Shanghai Jiao Tong University  800 Dongchuan Road 200230 Shanghai P.\u2005R. 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