Two-dimensional coordination polymers (CPs) have aroused tremendous interest as electrocatalysts because the catalytic performance could be fine-tuned by their well-designed coordination layers with highly accessible and active metal sites.However,it remains great challenge for CP-based catalysts to be utilized for electrocatalytic oxidation reactions due to their inefficient activities and low catalytic sta-bilities.Herein,we applied a mixed-metal strategy to fabricate two-dimensional CoxNi1-x-CPs with dual active sites for electrocatalytic water and urea oxidation.By metal ratio regulation in the two-dimensional layer,an optimized Co2/3Ni1/3-CP exhibits a water oxidation performance with an overpoten-tial of 325 mV at a current density of 10 mAcm-2 and a Tafel slope of 86 mV dec-1 in alkaline solution for oxygen evolution reaction.Importantly,a lower potential than that of commercial RuO2 is observed over 20 mA cm-2.Co2/3Ni1/3-CP also displays a potential of 1.381 V at 10 mA cm-2 for urea oxidation reaction and a Tafel slope of 124 mV dec-1.This mixed-metal strategy to maximize synergistic effect of different metal centers may ultimately lead to promising electrocatalysts for small molecule oxidation reaction.