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Here, time-resolved SAXS\/WAXS reveals the mechanism of aqueous NCA-ROPISA during \u03b3-benzyl-l-glutamate N-carboxyanhydride polymerization. Early nucleation of PEG-stabilized micelles creates nanoconfined reaction environments that favor polymerization by concentrating soluble monomers and maintaining reactive amino chain ends despite progressive acidification. Concurrently, \u03b2-sheet formation emerges at the onset of self-assembly, stabilizing nascent nuclei and directing anisotropic nanoparticle growth. These findings establish how nanoconfinement and secondary-structure formation cooperatively govern polymerization, self-assembly, and morphology development. Reminiscent of the ribosomal peptidyl transferase center, these self-generated nanoreactors exploit confinement to promote peptide-bond formation in water, identifying nanoconfinement as a general strategy for coupling polymerization, molecular folding, and self-assembly in biomimetic materials.<\/jats:p>","DOI":"10.1021\/acs.biomac.6c01726","type":"journal-article","created":{"date-parts":[[2026,9,28]],"date-time":"2026-09-28T18:02:36Z","timestamp":1790618556000},"page":"7007-7020","source":"Crossref","is-referenced-by-count":0,"title":["Mechanism of Aqueous NCA-ROPISA: Self-Generated Nanoreactors, Peptide Folding and Self-Assembly"],"prefix":"10.1021","volume":"27","author":[{"given":"Hannah","family":"Beauseroy","sequence":"first","affiliation":[{"name":"CNRS , 5629, ,","place":["Pessac, France, F-33600"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4466-5907","authenticated-orcid":true,"given":"Sifan","family":"Ji","sequence":"additional","affiliation":[{"name":"CNRS , 5629, ,","place":["Pessac, France, F-33600"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guillaume","family":"Fleury","sequence":"additional","affiliation":[{"name":"CNRS , 5629, ,","place":["Pessac, France, F-33600"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0752-8735","authenticated-orcid":true,"given":"Franck","family":"Wien","sequence":"additional","affiliation":[{"name":"Synchrotron SOLEIL , L\u2019Orme des Merisiers Gif-sur-Yvette , ,","place":["Saint Aubin, France, F-91410"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8779-7897","authenticated-orcid":true,"given":"Thomas","family":"Bizien","sequence":"additional","affiliation":[{"name":"Synchrotron SOLEIL , L\u2019Orme des Merisiers Gif-sur-Yvette , ,","place":["Saint Aubin, France, F-91410"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0952-1358","authenticated-orcid":true,"given":"Annie","family":"Bru\u0302let","sequence":"additional","affiliation":[{"name":"CEA-CNRS , , ,","place":["Gif-sur-Yvette, France, F-91191"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7213-7861","authenticated-orcid":true,"given":"Colin","family":"Bonduelle","sequence":"additional","affiliation":[{"name":"CNRS , 5629, ,","place":["Pessac, France, F-33600"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0465-8603","authenticated-orcid":true,"given":"Se\u0301bastien","family":"Lecommandoux","sequence":"additional","affiliation":[{"name":"CNRS , 5629, ,","place":["Pessac, France, F-33600"]},{"name":"Institut Universitaire de France (IUF) , 1 rue Descartes, Cedex 05 , ,","place":["Paris, France, 75231"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,28]]},"reference":[{"issue":"8","key":"2026101210565262700_cit1","doi-asserted-by":"publisher","first-page":"1029","DOI":"10.1021\/acsmacrolett.9b00464","article-title":"Emerging Trends in Polymerization-Induced Self-Assembly","volume":"8","author":"Penfold","year":"2019","journal-title":"ACS Macro Lett."},{"issue":"1","key":"2026101210565262700_cit2","doi-asserted-by":"publisher","DOI":"10.1002\/agt2.418","article-title":"Recent Progress in Polymerization-Induced Self-Assembly: From the Perspective of Driving Forces","volume":"5","author":"Zhao","year":"2024","journal-title":"Aggregate"},{"key":"2026101210565262700_cit3","doi-asserted-by":"publisher","first-page":"101637","DOI":"10.1016\/j.progpolymsci.2022.101637","article-title":"In Situ Encapsulation of Biologically Active Ingredients into Polymer Particles by Polymerization in Dispersed Media","volume":"137","author":"Lages","year":"2023","journal-title":"Prog. 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