Due to the significant relationships between structure and properties, the controlled construction of atomically precise metal clusters presents both a formidable challenge and great importance. The innovative synthesis of well-defined silver nanoclusters with near-infrared II (NIR-II) luminescent properties may inspire further exploration of functional metal nanoclusters for bioimaging applications. In this study, we employed the multidentate chelating nitrogen ligand 3,5-di(2-pyridyl)pyrazole (Hbpypz) to construct three unprecedented silver nanoclusters: [Ag(bpypz)] (), [Ag(bpypz)] (), and [Ag(bpypz)] (). Single-crystal X-ray analysis indicated that these cluster structures stem from Ag units, exhibiting cluster-of-cluster configurations. By modulating the stoichiometry of the chelating ligand and silver centers, we achieved controlled size growth and reversible cluster-to-cluster conversions among these silver nanoclusters. Notably, the nanocluster exhibits an interesting thermally activated delayed fluorescence (TADF) based luminescence in the second near-infrared (NIR-II) region and demonstrates high catalytic efficiency in the oxidative coupling of benzylamines via a singlet oxygen (O) oxidation mechanism.
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