“…The chemical composition and valence states of Mo 6 S 8 were further investigated by XPS (Figure S2). For the fine Mo 3d spectrum (Figure h), the peak at 226.1 eV corresponds to S 2s, and two asymmetric doublets located at 228.1/231.2 eV and 229.2/232.3 eV are attributed to Mo 3+ and Mo 2+ , respectively. , The presence of Mo 6+ (peaks positioned at 232.8 and 235.8 eV) could be ascribed to slight surface oxidation of the sample due to air contact. The high-resolution S 2p spectra can be fitted into three doublets at 160.8/162.0 eV, 161.8/163.0 eV, and 163.5/164.6 eV, which are assigned to 3-coordinated S 2– , 4-coordinated S 2– , and nonstoichiometric sulfur atoms from the extreme surface (Figure i). , In addition, the Raman spectrum of the Mo 6 S 8 sample (Figure S3) shows five obvious peaks at 136, 233, 316, 376, and 404 cm –1 , which are attributed to the various vibrational phonons of Mo/S and further confirm the well-established preparation of Mo 6 S 8 …”