Probing Edge Site Reactivity of Oxidic Cobalt Water Oxidation Catalysts

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Department of Chemistry and Chemical Biology, Harvard University, 12 Oxford Street, Cambridge, Massachusetts 02138, United States
Cite this: J. Am. Chem. Soc. 2016, 138, 12, 4229–4236
Publication Date (Web):February 24, 2016
Copyright © 2016 American Chemical Society
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Differential electrochemical mass spectrometry (DEMS) analysis of the oxygen isotopologues produced by 18O-labeled Co-OEC in H216O reveals that water splitting catalysis proceeds by a mechanism that involves direct coupling between oxygens bound to dicobalt edge sites of Co-OEC. The edge site chemistry of Co-OEC has been probed by using a dinuclear cobalt complex. 17O NMR spectroscopy shows that ligand exchange of OH/OH2 at Co(III) edge sites is slow, which is also confirmed by DEMS experiments of Co-OEC. In borate (Bi) and phosphate (Pi) buffers, anions must be displaced to allow water to access the edge sites for an O–O bond coupling to occur. Anion exchange in Pi is slow, taking days to equilibrate at room temperature. Conversely, anion exchange in Bi is rapid (kassoc = 13.1 ± 0.4 M–1 s–1 at 25 °C), enabled by facile changes in boron coordination. These results are consistent with the OER activity of Co-OEC in Bi and Pi. The Pi binding kinetics are too slow to establish a pre-equilibrium sufficiently fast to influence the oxygen evolution reaction (OER), consistent with the zero-order dependence of Pi on the OER current density; in contrast, Bi exchange is sufficiently facile such that Bi has an inhibitory effect on OER. These complementary studies on Co-OEC and the dicobalt edge site mimic allow for a direct connection, at a molecular level, to be made between the mechanisms of heterogeneous and homogeneous OER.

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  • Full experimental details, further DEMS data, crystallographic summary, pH titration data, 1H NMR spectra, Job plot, and electrochemical data (PDF)

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