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Homogeneous electrocatalytic proton reduction is reported using cobalt complex [ 1 ](BF 4 ) 2 . This complex comprises two bis(1‐methyl‐4,5‐diphenyl‐1 H ‐imidazol‐2‐yl)methane (HBMIMPh2) ligands that contain an acidic methylene moiety in their backbone. Upon reduction of [ 1 ](BF 4 ) 2  by either electrochemical or chemical means, one of its HBMIMPh2ligands undergoes deprotonation under the formation of dihydrogen. Addition of a mild proton source (acetic acid) to deprotonated complex [ 2 ](BF 4 ) regenerates protonated complex [ 1 ](BF 4 ) 2 . In presence of acetic acid in acetonitrile solvent [ 1 ](BF 4 ) 2  shows electrocatalytic proton reduction with a  k  obs  of ≈200 s −1  at an overpotential of 590 mV. Mechanistic investigations supported by DFT (BP86) suggest that dihydrogen formation takes place in an intramolecular fashion through the participation of a methylene C−H bond of the HBMIMPh2ligand and a Co II −H bond through formal heterolytic splitting of the latter. These findings are of interest to the development of responsive ligands for molecular (base)metal (electro)catalysis.

chemistry – a european journal

Electrocatalytic Proton Reduction by a Cobalt Complex Containing a Proton‐Responsive Bis(alkylimdazole)methane Ligand: Involvement of a C−H Bond in H 2  Formation