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Transition metal is known to influence electrochemical activities over transition metals (M) and nitrogen (N)-codoped carbon (Msingle bondNsingle bondC) catalysts. However, champion transition metals centers in Msingle bondNsingle bondC for catalyzing CO₂ reduction reaction (CO2RR) remain unclear, hindering further catalyst development with enhanced performance. Herein, we report the investigation of effects of five transition metals (Cr, Mn, Fe, Co, Ni) on CO2RR activities and mechanisms using metal-doped nitrogenated carbon nanosheets as model catalysts fabricated via a novel space-confinement-assisted molecular-level complexing approach. Analyzing N 1s XPS spectra confirmed the formation of M−N complexes via the coordination of metals atoms with pyridinic N, which was identified as the active species in CO2RR. According to activity descriptors including overpotentials, Faradaic efficiency (FE …