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Herein, we report the use of subcomponent self\u2010assembly for the construction of anion\u2010coordinated quadruple helicates with high to quantitative yields. These quadruple helicates were assembled in situ from simple subcomponents through the simultaneous formation of dynamic acylhydrazone bonds and hydrogen bonds. Among them, the A\n                    <jats:sub>2<\/jats:sub>\n                    <jats:bold>L<\/jats:bold>\n                    <jats:sub>4<\/jats:sub>\n                    quadruple helicate featuring linkers of 4,4\u2032\u2010methylenebis(phenyl) (\n                    <jats:bold>\n                      H\n                      <jats:sup>1<\/jats:sup>\n                    <\/jats:bold>\n                    ) demonstrated the ability to encapsulate a range of cationic guests, such as TBA\n                    <jats:sup>+<\/jats:sup>\n                    and TPA\n                    <jats:sup>+<\/jats:sup>\n                    . At the same time, the templating effect of the guests was able to drive the selective formation of\n                    <jats:bold>\n                      H\n                      <jats:sup>1<\/jats:sup>\n                    <\/jats:bold>\n                    \u2283TBA from a dynamic combinatorial library. Notably, the incorporated acylhydrazone units function as a photoresponsive motif, enabling light\u2010induced release of encapsulated guests. By demonstrating subcomponent self\u2010assembly for constructing photoresponsive anion\u2010coordinated architectures, this work provides a robust strategy that paves the way for metal\u2010free, high\u2010nuclearity hydrogen\u2010bonded assemblies and their advanced applications in smart materials for targeted molecular delivery and release.\n                  <\/jats:p>","DOI":"10.1002\/anie.9038203","type":"journal-article","created":{"date-parts":[[2026,9,9]],"date-time":"2026-09-09T04:11:35Z","timestamp":1788927095000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Subcomponent Self\u2010Assembly of Anion\u2010Coordinated Quadruple Helicates With Light\u2010Induced Guest Release"],"prefix":"10.1002","author":[{"given":"Leilei","family":"Xu","sequence":"first","affiliation":[{"name":"Key Laboratory of Synthetic and Natural Functional Molecule of the Ministry of Education College of Chemistry and Materials 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