Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character

Amtawong, Jaruwan; Balcells, David; Wilcoxen, Jarett; Handford, Rex C.; Biggins, Naomi; Nguyen, Andy I.; Britt, R. David; Tilley, T. Don

doi:10.1021/jacs.9b10320

Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal Ru^V–Oxo with Significant Oxyl Radical Character

Journal Article · Thu Nov 07 00:00:00 EST 2019 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.9b10320· OSTI ID:1779231

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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.

High-valent Ru^V-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 Co^II(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 [Ru^V(S = 1/2)Co^III3(S = 0)O₄] configuration and non-negligible covalency in the cubane core. Significant oxyl radical character in the Ru^V-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 Ru^V-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 Ru^V-oxo moiety via a strong π-electron donation.

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Research Organization:: Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)

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

Grant/Contract Number:: AC02-05CH11231

OSTI ID:: 1779231

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 50 Vol. 141; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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CCDC 1970792: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244ry0 The current record is supplemented by this dataset	dataset	January 2019
CCDC 1970793: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244rz1 The current record is supplemented by this dataset	dataset	January 2019
CCDC 1970794: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244s03 The current record is supplemented by this dataset	dataset	January 2019
CCDC 1970795: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244s14 The current record is supplemented by this dataset	dataset	January 2019
CCDC 1970796: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244s25 The current record is supplemented by this dataset	dataset	January 2019
CCDC 1970797: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244s36 The current record is supplemented by this dataset	dataset	January 2019
CCDC 1970798: Experimental Crystal Structure Determination Jaruwan, Amtawong,; David, Balcells,; Jarett, Wilcoxen, https://doi.org/10.5517/ccdc.csd.cc244s47 The current record is supplemented by this dataset	dataset	January 2019

Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal RuV–Oxo with Significant Oxyl Radical Character

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Isolation and Study of Ruthenium–Cobalt Oxo Cubanes Bearing a High-Valent, Terminal Ru^V–Oxo with Significant Oxyl Radical Character