Interrogating the photogenerated Ir(iv) state of a water oxidation catalyst using ultrafast optical and X-ray absorption spectroscopy

Vagnini, Michael T.; Mara, Michael W.; Harpham, Michael R.; Huang, Jier; Shelby, Megan L.; Chen, Lin X.; Wasielewski, Michael R.

doi:10.1039/c3sc51511g

Title: Interrogating the photogenerated Ir(iv) state of a water oxidation catalyst using ultrafast optical and X-ray absorption spectroscopy

Journal Article · Tue Jan 01 00:00:00 EST 2013 · Chemical Science

DOI:https://doi.org/10.1039/c3sc51511g· OSTI ID:1386097

Vagnini, Michael T.; Mara, Michael W.; Harpham, Michael R.; Huang, Jier; Shelby, Megan L.; Chen, Lin X.; Wasielewski, Michael R.

Using sunlight to drive molecular water oxidation catalysts for fuel formation requires understanding the single electron transfer events involved in catalyst activation. In an effort to photogenerate and characterize the highly reactive Ir(IV) state of the Ir(III)-based water oxidation catalyst Cp*Ir(ppy)Cl (ppy = 2-phenylpyridine), we have incorporated the complex into a covalent electron acceptor–chromophore–Cp*Ir(ppy)Cl triad, in which naphthalene-1,8:4,5-bis(dicarboximide) (NDI) is the electron acceptor and perylene-3,4-dicarboximide (PMI) is the chromophore. Photoexcitation of the PMI chromophore in dichloromethane results in two competitive reactions: NDI–1*PMI–Ir(III) → NDI–PMI˙-–Ir(IV) and NDI–1*PMI–Ir(III) → NDI˙-–PMI˙+–Ir(III) that each proceed with τ < 5 ps, as determined by femtosecond transient absorption spectroscopy. Both intermediate ion pairs undergo charge shift reactions to produce NDI˙-–PMI–Ir(IV). The fully charge-separated ion pair has a lifetime of 17.2 ± 0.1 ns, and its photophysical behavior is similar in the more polar solvent benzonitrile. Time-resolved X-ray absorption measurements on the triad at 100 ps following PMI photoexcitation show a new absorption feature at the LIII-edge of Ir and a blue-shifted white-line peak, which provides direct evidence of a change in the Ir oxidation state from Ir(III) to Ir(IV), consistent with the photophysical measurements. Our work underscores the utility of ultrafast spectroscopy performed on covalent assemblies of electron donor–acceptor systems with solar fuels catalysts to generate and probe their higher valence states in ways that complement chemical or electrochemical oxidation and establish the nature of key intermediates implicated in their catalytic mechanisms.

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Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Argonne-Northwestern Solar Energy Research Center (ANSER)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

DOE Contract Number:: SC0001059

OSTI ID:: 1386097

Journal Information:: Chemical Science, Vol. 4, Issue 10; Related Information: ANSER partners with Northwestern University (lead); Argonne National Laboratory; University of Chicago; University of Illinois, Urbana-Champaign; Yale University; ISSN 2041-6520

Publisher:: Royal Society of Chemistry

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
catalysis (homogeneous)
catalysis (heterogeneous)
solar (photovoltaic)
solar (fuels)
photosynthesis (natural and artificial)
bio-inspired
hydrogen and fuel cells
electrodes - solar
defects
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materials and chemistry by design
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Title: Interrogating the photogenerated Ir(iv) state of a water oxidation catalyst using ultrafast optical and X-ray absorption spectroscopy

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