Determining the structures of nanoparticles at atomic resolution is vital to understand theirstructure–property correlations. Large metal nanoparticles with core diameter beyond 2 nmhave, to date, eluded characterization by single-crystal X-ray analysis. Here we report thechemical syntheses and structures of two giant thiolated Ag nanoparticles containing 136 and374 Ag atoms (that is, up to 3 nm core diameter). As the largest thiolated metal nanoparticlescrystallographically determined so far, these Ag nanoparticles enter the trulymetallic regime with the emergence of surface plasmon resonance. As miniatures of fivefoldtwinned nanostructures, these structures demonstrate a subtle distortion within fivefoldtwinned nanostructures of face-centred cubic metals. The Ag nanoparticles reported in thiswork serve as excellent models to understand the detailed structure distortion within twinnedmetal nanostructures and also how silver nanoparticles can span from the molecular to themetallic regime.
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