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Herein, we demonstrate the rapid generation (\n                    <jats:italic>t<\/jats:italic>\n                    \u2264 5 min) of size\u2010tunable ultralow dispersity (\n                    <jats:italic>\u00d0<\/jats:italic>\n                    \u2264 1.01) 2D hexagonal nanosheets governed by self\u2010limiting self\u2010assembly (SLSA). Self\u2010assembly in natural systems occurs with exquisite control of structure, function, and dimension. We demonstrate that key aspects of biological assembly can be rationally applied toward the development of bottom\u2010up approaches for the construction of chiral nanomaterials. To this end, self\u2010limiting polymerization\u2010induced crystallization\u2010driven self\u2010assembly (SL\u2010PI\u2010CDSA) of modular and templating aryl isocyanide (AIC) monomers yields functional 2D assemblies permitting post\u2010polymerization\/assembly modifications. Detailed study of the internal and external structure of the hexagonal nanosheets reveals topological defects which offer mechanistic insights into both their assembly and subsequent utilization. Specifically, these features enable fabrication of chiral hybrid organic\u2013inorganic nanomaterials incorporating chiral plasmonic metal nanoparticles (MNPs). Our results suggest that the synergistic interplay of template\u2010driven confinement and hierarchical chirality induce symmetry breaking of in situ\u2010generated gold MNPs. We anticipate that the platform presented will facilitate fabrication of new hybrid, chiral organic\u2013inorganic nanostructures.\n                  <\/jats:p>","DOI":"10.1002\/anie.7896560","type":"journal-article","created":{"date-parts":[[2026,4,17]],"date-time":"2026-04-17T05:28:11Z","timestamp":1776403691000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Self\u2010Limiting Polymerization\u2010Induced Crystallization\u2010Driven Self\u2010Assembly (SL\u2010PI\u2010CDSA) Enables Templated Synthesis of Chiral Plasmonic, Hybrid 2D Hexagonal Assemblies"],"prefix":"10.1002","volume":"65","author":[{"given":"Randall A.","family":"Scanga","sequence":"first","affiliation":[{"name":"Department of Chemistry University of Massachusetts Lowell  Lowell Massachusetts USA"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Sean H.","family":"Sarault","sequence":"additional","affiliation":[{"name":"Department 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