Co–N–C catalysts are promising candidates for substituting platinum in electrocatalysis and organic transformations. The heterogeneity of the Co species resulting from high-temperature pyrolysis, however, encumbers the structural identification of active sites. Herein, we report a self-supporting Co–N–C catalyst wherein cobalt is dispersed exclusively as single atoms. By using sub-Ångström-resolution HAADF-STEM in combination with XAFS and DFT calculation, the exact structure of the Co–N–C is identified to be CoN4C8-1-2O2, where the Co center atom is coordinated with four pyridinic N atoms in the graphitic layer, while two oxygen molecules are weakly adsorbed on Co atoms in perpendicular to the Co–N4 plane. This single-atom dispersed Co–N–C catalyst presents excellent performance for the chemoselective hydrogenation of nitroarenes to produce azo compounds under mild reaction conditions.
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