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Herein, we report a supramolecular cage system showing substituent-directed topology redistribution and fluorescence modulation under acid\/base regulation. Acid- and base-induced ring-closing and ring-opening reactions provide a covalent structural switch in bisimidazolium ligands, and the resulting ligands self-assemble with Zn2+ ions into cage assemblies assigned to cuboctahedral, octahedral, square-prismatic, and triangular-prismatic cage architectures. The steric hindrance and spatial orientation of the substituents modulate the apparent cage topology distribution, while coordination-induced cage rigidity and substituent-dependent local steric restriction jointly give rise to fluorescence modulation with quantum yields varying by more than two orders of magnitude. Furthermore, the hierarchical self-assembly of cuboctahedral cages into hexagonal nanoaggregates or lyotropic nanostructures was observed by TEM, depending on the electrostatics and geometry-induced packing forces. This study demonstrates how substituent-directed ligand design couples acid-\/base-responsive cage topology redistribution with optical and aggregation behaviors.<\/jats:p>","DOI":"10.1021\/acsami.6c09202","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T14:40:10Z","timestamp":1785854410000},"page":"44302-44312","source":"Crossref","is-referenced-by-count":0,"title":["Acid-\/Base- and Site-Hindrance-Induced Cage Transformation and Hierarchical Self-Assembly of Regular Nanoaggregates"],"prefix":"10.1021","volume":"18","author":[{"given":"Miao","family":"Li","sequence":"first","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yu-Qi","family":"Shi","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tianyu","family":"Guo","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Longbin","family":"Su","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chuangwei","family":"Zhou","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Qixia","family":"Bai","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hong-Fei","family":"Pan","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8721-6167","authenticated-orcid":true,"given":"Tun","family":"Wu","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8743-3794","authenticated-orcid":true,"given":"Zhe","family":"Zhang","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8287-1410","authenticated-orcid":true,"given":"Pei-Yang","family":"Su","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-6717-7642","authenticated-orcid":true,"given":"Ting-Zheng","family":"Xie","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-1988-7604","authenticated-orcid":true,"given":"Pingshan","family":"Wang","sequence":"additional","affiliation":[{"name":"Ministry of Education; Guangzhou University , , ,","place":["Guangzhou, China, 510006"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,4]]},"reference":[{"key":"2026081905151969500_cit1","doi-asserted-by":"publisher","first-page":"157","DOI":"10.1016\/j.bbrc.2008.01.057","article-title":"Regulation of the Function of Mammalian Myosin and Its Conformational Change","volume":"369","author":"Ikebe","year":"2008","journal-title":"Biochem. 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