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However, the inherent complexity of supramolecular systems presents significant challenges for real\u2010time visualization, particularly in capturing the growth kinetics of individual assemblies and the hierarchical formation of network structures at the single\u2010assembly level. Here, we visualized the dynamic growth and network formation of benzyl\u2010naphthalimide dye assemblies in situ by confocal laser scanning microscopy (CLSM). In situ time\u2010lapse imaging revealed distinct dynamic growth mechanisms among the three assemblies. Theoretical calculations demonstrated that different amino substituents significantly influenced assembly morphologies by modulating the planarity of the naphthalene ring. Furthermore, fluorescence lifetime imaging revealed pronounced intra\u2010assembly heterogeneity, highlighting diverse molecular packing arrangements within individual assemblies. The confocal in situ visualization technique provided single\u2010assembly growth dynamics, offering insights unattainable through conventional spectroscopic methods. Our work reveals that naphthalimide\u2010based molecules can self\u2010assemble into a variety of distinct architectures, underscoring their potential for designing advanced functional materials with tunable properties.<\/jats:p>","DOI":"10.1002\/chem.202500979","type":"journal-article","created":{"date-parts":[[2025,4,23]],"date-time":"2025-04-23T03:44:58Z","timestamp":1745379898000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["In Situ Real\u2010Time Imaging of Benzyl\u2010Naphthalimide Dyes Revealing Diverse Structural Evolution Dynamics at the Single\u2010Assembly Level"],"prefix":"10.1002","volume":"31","author":[{"given":"Yinchan","family":"Zhang","sequence":"first","affiliation":[{"name":"Dalian Institute of Chemical Physics Chinese Academy of Sciences  457 Zhongshan Road Dalian 116023 China"},{"name":"University of Chinese Academy of Sciences  Beijing 100049 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