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A number of polycrystalline copper(I) O,O′‐dialkyldithiophosphate cluster compounds with Cu4, Cu6, and Cu8cores were synthesized and characterized by using extended X‐ray absorption fine‐structure (EXAFS) spectroscopy. The structural relationship of these compounds is discussed. The polycrystalline copper(I) O,O′‐diisobutyldithiophosphate cluster compounds, [Cu8{S2P(OiBu)2}6(S)] and [Cu6{S2P(OiBu)2}6], were also characterized by using 31P CP/MAS NMR (CP = cross polarization, MAS = magic‐angle spinning) and static 65Cu NMR spectroscopies (at different magnetic fields) and powder X‐ray diffraction (XRD) analysis. Comparative analyses of the 31P chemical‐shift tensor, and the 65Cu chemical shift and quadrupolar‐splitting parameters, estimated from the experimental NMR spectra of the polycrystalline copper(I) cluster compounds, are presented. The adsorption mechanism of the potassium O,O′‐diisobutyldithiophosphate collector, K[S2P(OiBu)2], at the surface of synthetic chalcocite (Cu2S) was studied by means of solid‐state 31P CP/MAS NMR spectroscopy and scanning electron microscopy (SEM). 31P NMR resonance lines from collector‐treated chalcocite surfaces were assigned to a mixture of [Cu8{S2P(OiBu)2}6(S)] and [Cu6{S2P(OiBu)2}6] compounds.