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Summary: Single-atom catalysts (SACs) have promising atomic utilization efficiency and catalytic activity, but their construction with a specific coordination mode remains challenging. This protocol describes the synthesis of a coordinated Fe-SAC@COF for boosted electrocatalytic oxygen evolution reaction (OER). We also detail the steps for single iron atoms confinement and characterization of the COF and Fe-SAC@COF with X-ray diffraction and transmission electron microscopy technique.For complete details on the use and execution of this protocol, please refer to Wang et al. (2022). : Publisher’s note: Undertaking any experimental protocol requires adherence to local institutional guidelines for laboratory safety and ethics.