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Electrochemical water reduction by employing first‐row transition‐metal nanoparticles (NPs) constitutes a sustainable way for the generation of H2. We have synthesized Co‐based NPs from a molecular CoII/CoIII precursor after its reductive decomposition at –1.86 V versus NHE in different organic solvents. These NPs are able to electrochemically reduce water at pH 14. SEM, EDX and XPS analyses have...
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