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Nanoclusters (NCs) bridge the gap between atoms and nanomaterials in not only dimension but also physicochemical properties. Precise chemical and structural control, as well as clear understanding of formation mechanisms, have been important to fabricate NCs with high performance in optoelectronics, catalysis, nanoalloys, and energy conversion and harvesting. Herein, taking advantage of the close chemical properties of Ln 3+  (Ln = Eu, Nd, Sm, Gd, etc.) and Gd 3+ –Eu 3+  energy transfer ion-pair, we report a clickable LnF 3  nanoparticle assembly strategy allowing reliable fabrication of diversely structured NCs, including single-component, dimeric, core-shelled/core-shell-shelled, and reversely core-shelled/core-shell-shelled, particularly with synergized optical functionalities. Moreover, the purposely-embedded dual luminescent probes offer great superiority for in situ and precise tracking of tiny structural variations and energy transfer pathways within complex nanoarchitectures.

A luminescent view of the clickable assembly of LnF3 nanoclusters