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For this study, we designed structurally defined bicyclic monomers in which the \u03b2 subunits in two Hb molecules are bridged through four-armed PEG of different molecular weights (10 and 40 kDa). These bicyclic monomers undergo concentration-dependent supramolecular ring-opening polymerization, enabling predictable control of polymer structure from discrete monomers to polymer particles and finally to a percolated polymer gel network. Extensive physicochemical analyses revealed quantitative shifts in polymerization equilibria that govern these supramolecular assemblies. Furthermore, intramolecular \u03b2\u03b2-cross-linking of Hb moiety with bis-(3,5-dibromosalicyl) fumarate (DBBF) allowed selective covalent fixation of each supramolecular polymer species, affording fixed bicyclic monomers, fixed polymer particles, and fixed polymer gels with controlled sizes. These fixed Hb\u2212PEG architectures retained characteristic O2-binding properties. Overall, this work establishes a supramolecular-to-covalent polymer conversion platform that enables precise structural control in Hb-based polymer architectures, thereby expanding the design space for protein\u2212polymer biomaterials.<\/jats:p>","DOI":"10.1021\/acs.biomac.6c01459","type":"journal-article","created":{"date-parts":[[2026,9,30]],"date-time":"2026-09-30T16:03:18Z","timestamp":1790784198000},"page":"6840-6852","source":"Crossref","is-referenced-by-count":0,"title":["Supramolecular Hemoglobin\u2212PEG Polymerization Equilibria as the Structural Basis for Providing Size-Controlled Polymer Particles"],"prefix":"10.1021","volume":"27","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-2429-9847","authenticated-orcid":true,"given":"Takashi","family":"Matsuhira","sequence":"first","affiliation":[{"name":"Nara Medical University , , 88 Shijo-cho , , ,","place":["Kashihara, Nara, Japan, 634-0813"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Masahiro","family":"Nagao","sequence":"additional","affiliation":[{"name":"Nara Medical University , , 88 Shijo-cho , , ,","place":["Kashihara, Nara, Japan, 634-0813"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6622-4934","authenticated-orcid":true,"given":"Yuki","family":"Nakano","sequence":"additional","affiliation":[{"name":"Anton Paar Japan K.K , 1-19-9 Tsutsumi-dori , , ,","place":["Sumida-ku, Tokyo, Japan, 131-0034"]},{"name":". , 1-19-9 Tsutsumi-dori , , ,","place":["Sumida-ku, Tokyo, Japan, 131-0034"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-0681-3032","authenticated-orcid":true,"given":"Hiromi","family":"Sakai","sequence":"additional","affiliation":[{"name":"Nara Medical University , , 88 Shijo-cho , , ,","place":["Kashihara, Nara, Japan, 634-0813"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,30]]},"reference":[{"issue":"11","key":"2026101210563043000_cit1","doi-asserted-by":"publisher","first-page":"1304","DOI":"10.1002\/anie.199013041","article-title":"Perspectives in supramolecular chemistry \u2212 from molecular recognition towards molecular information processing and self-organization","volume":"29","author":"Lehn","year":"1990","journal-title":"Angew. 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