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Multicomponent supramolecular assembly systems enable the generation of materials with outstanding properties, not obtained from single‐component systems, via a synergetic effect. Herein, we demonstrate a novel supramolecular coassembly system rendering highly ordered quantum dot (QD) arrangement structures formed via the self‐assembly of azobenzene derivatives, where the photocontrollable photoluminescence (PL) properties of the QDs are realized based on photoisomerization. Upon mixing the assembled azobenzene derivatives and QDs in apolar media, a time‐evolution coaggregation into hierarchical nanosheets with a highly ordered QD arrangement structure occurs. Upon photoirradiation, the nanosheets transform into ill‐defined aggregates without arranged QDs together with enhancing the PL intensity. In days, the photoirradiated coaggregates undergo recovery of the PL properties corresponding to the arranged QDs through thermal isomerization.

The formation of well-defined nanostructures comprising assembled semiconductor quantum dots (QDs) is a challenging research task. Recently, we found that the introduction of π-conjugated molecules with a self-assembly ability into small CdSe QDs led to the formation of highly ordered QD arrangements. Here, we demonstrate the in-depth coaggregation process of large-sized CdSe QDs and azobenzene derivative 1 possessing an amino group functioning as an adhesive to the QD surface. Upon mixing the above QDs with assembled azobenzene derivative 1 in apolar solvents, linearly arranged QD structures along assembled azobenzene derivative 1 were formed over time. In the formed coaggregates, efficient energy transfer between the arranged QDs occurred, as confirmed by a change in the emission spectra and lifetimes. Analysis of time-dependent emission properties revealed the coaggregation mechanism of QDs and 1.