A Uranium(II) Arene Complex That Acts as a Uranium(I) Synthon

Straub, Mark D.; Ouellette, Erik T.; Boreen, Michael A.; Britt, R. David; Chakarawet, Khetpakorn; Douair, Iskander; Gould, Colin A.; Maron, Laurent; Del Rosal, Iker; Villarreal, David; Minasian, Stefan G.; Arnold, John

doi:10.1021/jacs.1c07854

Title: A Uranium(II) Arene Complex That Acts as a Uranium(I) Synthon

Journal Article · 16 November 2021 · Journal of the American Chemical Society

DOI: https://doi.org/10.1021/jacs.1c07854 · OSTI ID:1863926

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Univ. of California, Berkeley, CA (United States); Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)
Univ. of California, Davis, CA (United States)
Univ. of Toulouse (France)
Univ. of California, Berkeley, CA (United States)

We report two-electron reduction of the amidate-supported U(III) mono(arene) complex U(TDA)₃ (2) with KC₈ yields the anionic bis(arene) complex [K[2.2.2]cryptand][U(TDA)₂] (3) (TDA = N-(2,6-di-isopropylphenyl)pivalamido). EPR spectroscopy, magnetic susceptibility measurements, and calculations using DFT as well as multireference CASSCF methods all provide strong evidence that the electronic structure of 3 is best represented as a 5f⁴ U(II) metal center bound to a monoreduced arene ligand. Reactivity studies show 3 reacts as a U(I) synthon by behaving as a two-electron reductant toward I₂ to form the dinuclear U(III)–U(III) triiodide species [K[2.2.2]cryptand][(UI(TDA)₂)₂(μ-I)] (6) and as a three-electron reductant toward cycloheptatriene (CHT) to form the U(IV) complex [K[2.2.2]cryptand][U(η⁷-C₇H₇)(TDA)₂(THF)] (7). The reaction of 3 with cyclooctatetraene (COT) generates a mixture of the U(III) anion [K[2.2.2]cryptand][U(TDA)₄] (1-crypt) and U(COT)₂, while the addition of COT to complex 2 instead yields the dinuclear U(IV)–U(IV) inverse sandwich complex [U(TDA)₃]₂(μ-η⁸:η³-C₈H₈) (8). Two-electron reduction of the homoleptic Th(IV) amidate complex Th(TDA)₄ (4) with KC₈ gives the mono(arene) complex [K[2.2.2]cryptand][Th(TDA)₃(THF)] (5). The C–C bond lengths and torsion angles in the bound arene of 5 suggest a direduced arene bound to a Th(IV) metal center; this conclusion is supported by DFT calculations.

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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). Chemical Sciences, Geosciences & Biosciences Division; USDOE National Nuclear Security Administration (NNSA); National Science Foundation (NSF); National Institutes of Health (NIH)

Grant/Contract Number:: AC02-05CH11231; NA0003180; NA0000979

OSTI ID:: 1863926

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 47 Vol. 143; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
uranium
arene
amidate
actinide

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Title: A Uranium(II) Arene Complex That Acts as a Uranium(I) Synthon

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