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Aggregation-induced emission (AIE) is an attractive strategy for enhancing the luminescence of metal nanoclusters (NCs). However, rational control of the AIE of Au NCs is currently one of the key challenges and fundamental understanding of the complex surface/interfacial structures, and the emission mechanism of AIE-type Au NCs is far from complete. In this study, we report a pH-controllable AIE accompanied with a self-assembly/disassembly process of Au NCs with Au(I)–thiolate complexes with glutathione (GSH)-protected AIE-type Au NCs as a model. It was found that the solution pH could be used to control the landscape of the Au(I)–thiolate complexes encapsulating the Au NCs, generating varied AIE. Transmission electron microscopy (TEM) studies revealed that the Au NCs were essentially embedded inside the pH-sensitive supramolecular assemblies of the Au(I)–thiolate complexes. It was further found …