Co/Co9S8 nanoparticles encapsulated in a N, S, and O ternary-doped carbon matrix were synthesized utilizing a Co-NSOMOF as a single precursor, and they exhibited excellent bifunctional electrocatalytic activity for the OER and HER. Impressively, the water splitting cell exhibited a low cell voltage of 1.56 V at 10 mA cm-2. The high performances were attributed to the synergistic effect and the protection of multi-heteroatom doped carbon shells for active Co/Co9S8 nanoparticles.