We report ultra-wideline, high-field natural abundance solid-state 33S NMR spectra of the Li-ion battery conversion electrode NbS3, the first 33S NMR study of a compound containing disulfide (S22-) units. The large quadrupolar coupling parameters (CQ ≈ 31 MHz) are consistent with values obtained from DFT calculations, and the spectra provide evidence for the linear Peierls distortion that doubles the number of 33S sites
