Recently, metal-organic frameworks (MOFs) with transition metal sulfides have gained much attention as electrode materials for supercapacitors (SCs). In this work, 3D-NCMOF@MS NCs, incorporating two-dimensional molybdenum disulphide (2D-MS) nanosheets and three-dimensional nickel cobalt-MOF nanocubes (3D-NCMOF NCs) are synthesized by a solvothermal and precipitation process. Owing to their enhanced electrical conductivity and huge surface area, the 3D-NCMOF@MS NCs produce superior electrochemical responses in SCs compared to 2D-MS and 3D-NCMOF NCs. The results demonstrate that the synergistic 3D-NCMOF@MS NCs increased specific capacitance up to 1048 Fg−1 at 1 Ag−1, revealing outstanding cycle stability with a capacitance retention of 99.06 %. Besides, the exposed high-power density of 3D-NCMOF@MS NCs reached 400 W kg−1 as well as an outstanding maximum energy density of 188.64 Wh kg−1. Such synergistic effects of the multivalent states of Ni, Co, and Mo promote electrochemical characteristics, implying that the 3D-NCMOF@MS NCs could potentially be used in energy storage systems, boosting electrochemical performance.