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Hydrogen Evolution Electrocatalysis with a Molecular Cobalt Bis(alkylimidazole)methane Complex in DMF: a critical activity analysis

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[Co(HBMIM Ph2 ) 2 ](BF 4 ) 2 ( 1 ), (HBMIM Ph2 = bis(1-methyl-4,5-diphenyl-1 H -imidazol-2-yl)methane), was investigated for its electrocatalytic hydrogen evolution performance in DMF using voltammetry and during controlled potential/current electrolysis (CPE/CCE) in a novel in-line product detection setup. Performances were benchmarked against three reported molecular cobalt HER electrocatalysts: [Co(dmgBF 2 ) 2 (solv) 2 ] ( 2 ), (dmgBF 2 = difluoroboryldimethylglyoximato), [Co(TPP)] ( 3 ), (TPP = 5,10,15,20-tetraphenylporphyrinato) and [Co(bapbpy)Cl](Cl) ( 4 ), (bapbpy = 6,6’-bis-(2-aminopyridyl)-2,2’-bipyridine) showing distinct performances differences with 1 being the runner up in H 2 evolution during CPE and the best catalyst in terms of overpotential and FE during CCE. After bulk electrolysis with all of the complexes a deposit on the glassy carbon electrode was observed and post electrolysis XPS analysis of the deposit formed from 1 demonstrated only a minor cobalt contribution (0.23%), mainly consisting of Co 2+ . Rinse tests on the deposits derived from 1 and 2 showed that the initially observed distinct activity is (partly) preserved for the deposits. These observations indicate that the molecular design of the complexes dictates the features of the formed deposit and therewith the observed activity.

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