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Comprehensive Summary: Metal organic frameworks have been employed as high‐performance layered double hydroxide (LDH) composite supercapacitor electrode materials but have shown unsatisfactory redox ability and stability. Herein, a host‐guest CuMo‐based polyoxometalate‐based metal organic framework (POMOF) with copious electrochemically active sites and strong electrochemical redox activities has been effectively coupled with POM‐incorporated CoNi‐LDH to develop a nanocomposite (NENU‐5@CoNi‐LDH) by a simple solvothermal method. The designed electrode shows a high specific capacity of 333.61 mAh·g–1 at 1 A·g–1. In addition, the novel hybrid symmetric supercapacitor NENU‐5@CoNi‐LDH/active carbon (AC) demonstrated a high energy density of 80.8 Wh·kg–1 at a power density of 750.7 W·kg–1. Interestingly, the nanocomposite of NENU‐5@CoNi‐LDH exhibits an outstanding capacitance retention of 79% after 5000 charge‐discharge cycles at 10 A·g–1. This work provides a new strategy and will be the backbone for future energy storage research. [ABSTRACT FROM AUTHOR]

Comprehensive Summary: Metal organic frameworks have been employed as high‐performance layered double hydroxide (LDH) composite supercapacitor electrode materials but have shown unsatisfactory redox ability and stability. Herein, a host‐guest CuMo‐based polyoxometalate‐based metal organic framework (POMOF) with copious electrochemically active sites and strong electrochemical redox activities has been effectively coupled with POM‐incorporated CoNi‐LDH to develop a nanocomposite (NENU‐5@CoNi‐LDH) by a simple solvothermal method. The designed electrode shows a high specific capacity of 333.61 mAh·g–1 at 1 A·g–1. In addition, the novel hybrid symmetric supercapacitor NENU‐5@CoNi‐LDH/active carbon (AC) demonstrated a high energy density of 80.8 Wh·kg–1 at a power density of 750.7 W·kg–1. Interestingly, the nanocomposite of NENU‐5@CoNi‐LDH exhibits an outstanding capacitance retention of 79% after 5000 charge‐discharge cycles at 10 A·g–1. This work provides a new strategy and will be the backbone for future energy storage research. [ABSTRACT FROM AUTHOR]