Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character
Abstract
High-valent RuV-oxo intermediates have long been proposed in catalytic oxidation chemistry, but investigations into their electronic and chemical properties have been limited due to their reactive nature and rarity. The incorporation of Ru into the [Co3O4] subcluster via the single-step assembly reaction of CoII(OAc)2(H2O)4 (OAc = acetate), perruthenate (RuO4-), and pyridine (py) yielded an unprecedented Ru(O)Co3(μ3-O)4(OAc)4(py)3 cubane featuring an isolable, yet reactive, RuV-oxo moiety. EPR, ENDOR, and DFT studies reveal a valence-localized [RuV(S = 1/2)CoIII3(S = 0)O4] configuration and non-negligible covalency in the cubane core. Significant oxyl radical character in the RuV-oxo unit is experimentally demonstrated by radical coupling reactions between the oxo cubane and both 2,4,6-tri-tert-butylphenoxyl and trityl radicals. The oxo cubane oxidizes organic substrates and, notably, reacts with water to form an isolable μ-oxo bis-cubane complex [(py)3(OAc)4Co3(μ3-O)4Ru]-O-[RuCo3(μ3-O)4(OAc)4(py)3]. Redox activity of the RuV-oxo fragment is easily tuned by the electron-donating ability of the distal pyridyl ligand set at the Co sites demonstrating strong electronic communication throughout the entire cubane cluster. Natural bond orbital calculations reveal cooperative orbital interactions of the [Co3O4] unit in supporting the RuV-oxo moiety via a strong π-electron donation.
- Authors:
-
[1];
[2];
[3];
[1];
[1];
[4];
[1];
[4]
- Univ. of California, Berkeley, CA (United States). Dept. of Chemistry
- Univ. of Oslo (Norway). Dept. of Chemistry, Hylleraas Centre for Quantum Molecular Sciences
- Univ. of California, Davis, CA (United States). Dept. of Chemistry
- Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Div.
- Publication Date:
- Research Org.:
- Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1779231
- Grant/Contract Number:
- AC02-05CH11231
- Resource Type:
- Accepted Manuscript
- Journal Name:
- Journal of the American Chemical Society
- Additional Journal Information:
- Journal Volume: 141; Journal Issue: 50; Journal ID: ISSN 0002-7863
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Redox reactions; Ligands; Oxidation; Quantum mechanics; Reactivity
Citation Formats
Amtawong, Jaruwan, Balcells, David, Wilcoxen, Jarett, Handford, Rex C., Biggins, Naomi, Nguyen, Andy I., Britt, R. David, and Tilley, T. Don. Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character. United States: N. p., 2019.
Web. doi:10.1021/jacs.9b10320.
Amtawong, Jaruwan, Balcells, David, Wilcoxen, Jarett, Handford, Rex C., Biggins, Naomi, Nguyen, Andy I., Britt, R. David, & Tilley, T. Don. Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character. United States. https://doi.org/10.1021/jacs.9b10320
Amtawong, Jaruwan, Balcells, David, Wilcoxen, Jarett, Handford, Rex C., Biggins, Naomi, Nguyen, Andy I., Britt, R. David, and Tilley, T. Don. Thu .
"Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character". United States. https://doi.org/10.1021/jacs.9b10320. https://www.osti.gov/servlets/purl/1779231.
@article{osti_1779231,
title = {Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character},
author = {Amtawong, Jaruwan and Balcells, David and Wilcoxen, Jarett and Handford, Rex C. and Biggins, Naomi and Nguyen, Andy I. and Britt, R. David and Tilley, T. Don},
abstractNote = {High-valent RuV-oxo intermediates have long been proposed in catalytic oxidation chemistry, but investigations into their electronic and chemical properties have been limited due to their reactive nature and rarity. The incorporation of Ru into the [Co3O4] subcluster via the single-step assembly reaction of CoII(OAc)2(H2O)4 (OAc = acetate), perruthenate (RuO4-), and pyridine (py) yielded an unprecedented Ru(O)Co3(μ3-O)4(OAc)4(py)3 cubane featuring an isolable, yet reactive, RuV-oxo moiety. EPR, ENDOR, and DFT studies reveal a valence-localized [RuV(S = 1/2)CoIII3(S = 0)O4] configuration and non-negligible covalency in the cubane core. Significant oxyl radical character in the RuV-oxo unit is experimentally demonstrated by radical coupling reactions between the oxo cubane and both 2,4,6-tri-tert-butylphenoxyl and trityl radicals. The oxo cubane oxidizes organic substrates and, notably, reacts with water to form an isolable μ-oxo bis-cubane complex [(py)3(OAc)4Co3(μ3-O)4Ru]-O-[RuCo3(μ3-O)4(OAc)4(py)3]. Redox activity of the RuV-oxo fragment is easily tuned by the electron-donating ability of the distal pyridyl ligand set at the Co sites demonstrating strong electronic communication throughout the entire cubane cluster. Natural bond orbital calculations reveal cooperative orbital interactions of the [Co3O4] unit in supporting the RuV-oxo moiety via a strong π-electron donation.},
doi = {10.1021/jacs.9b10320},
journal = {Journal of the American Chemical Society},
number = 50,
volume = 141,
place = {United States},
year = {Thu Nov 07 00:00:00 EST 2019},
month = {Thu Nov 07 00:00:00 EST 2019}
}
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