The self-assembly of mechanoluminochromic polynuclear gold­(I) complexes has attracted more and more attention in the field of supramolecular gold­(I) chemistry. In this work, we adopted a stepwise self-assembly strategy to precisely synthesize two polynuclear gold­(I) supramolecular clusters. Through cooperative AuI···AuI and Au–N interactions, the gold­(I) clusters 1 +•BF4 – and 2 4+•4BF4 – with Au4 and Au16 cores, respectively, were successfully constructed. In these supramolecular clusters, (dppm)­Au2Cl2 coordination motifs and trithiocyanuric linkers were stepwise assembled via sequential thiolate–chloride/phosphine coordination substitution and Au–S/Au–N coordination bond rearrangement. Two well-defined gold­(I) supramolecular clusters displayed intense emission both in the solid state and in solution. Furthermore, the ladder-shaped cluster 2 4+•4BF4 – exhibited reversible mechanochromic luminescence behavior in the solid state as well as aggregation-caused redshifted emission in solution. Upon mechanical grinding, the emission of the cluster 2 4+•4BF4 – changed from yellow at 582 nm to red at 612 nm. The initial emission could be fully recovered by treatment with acetonitrile.

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