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• W3030254865 abstract "Examples of transition metal complexes capable of the dual roles of light harvesting and catalysis of CO2 reduction are rare. This self-sensitized approach simplifies systems and efficiencies; therefore, complete understanding of mechanistic principles is essential for improving catalysts. Here, we present a comprehensive study of dark reactions using electrochemical techniques to understand the multiple pathways for the selective reduction of CO2 to CO by an example self-sensitized photocatalyst: [Ir(bip)(ppy)(CH3CN)]2+ (bip = 2,6-bis(benzimidazole)pyridine, ppy = 2-phenylpyridine). Cyclic voltammetry (CV) in acetonitrile under anhydrous conditions reveals electrocatalysis by a two electron cycle at −1.7 V vs Fc+/0 (denoted the cat-1 region) in which the metallocarboxylate formed by binding of Ir(I) to CO2 is cleaved by CO2 as the oxide acceptor. At −1.9 V (denoted the cat-2 region), the Ir(CO2) intermediate is reduced and catalysis is accelerated. In the presence of water, Ir(CO2) is protonated to Ir(CO2H), which is reduced at a potential less negative than −1.7 V, and then, the oxide acceptor is either CO2 to form HCO3– or protons to release H2O and the conjugate base of the acid source. Further reduction of Ir(CO2H) at cat-2 again accelerates catalysis. Rates vary widely in these various regimes with the minimum kobs of 0.3 s–1 for anhydrous cat-1 to a maximum cat-2 rate of 2100 s–1 with 1% water. Competitive deactivation pathways were discovered as Ir–Ir dimerization without reacting with CO2 or the formation of a hydride-bridged dinuclear complex during extended electrolysis at a high water concentration. The Ir–Ir dimer was characterized by high resolution mass spectrometry and X-ray absorption spectroscopy (XAS)." @default.
• W3030254865 created "2020-06-05" @default.
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• W3030254865 date "2020-05-27" @default.
• W3030254865 modified "2023-10-18" @default.
• W3030254865 title "Comprehensive Mechanisms of Electrocatalytic CO₂ Reduction by [Ir(bip)(ppy)(CH₃CN)](PF₆)₂" @default.
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• W3030254865 doi "https://doi.org/10.1021/acscatal.9b04371" @default.
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