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Aryl Nitrenium and Oxenium Ions with Unusual High-Spin π,π* Ground States: Exploiting (Anti)Aromaticity
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    Aryl Nitrenium and Oxenium Ions with Unusual High-Spin π,π* Ground States: Exploiting (Anti)Aromaticity
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    Department of Chemistry, Iowa State University, 2101 Hach Hall, Ames, Iowa 50010, United States
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    The Journal of Organic Chemistry

    Cite this: J. Org. Chem. 2017, 82, 24, 13550–13556
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    https://doi.org/10.1021/acs.joc.7b02698
    Published October 31, 2017
    Copyright © 2017 American Chemical Society

    Abstract

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    Nitrenium and oxenium ions are important reactive intermediates in synthetic and biological processes, and their ground electronic configurations are of great interest due to having distinct reactivities and properties. In general, the closed-shell singlet state of these intermediates usually react as electrophiles, while reactions of the triplet states of these ions react like typical diradicals (e.g., H atom abstractions). Nonsubstituted phenyl nitrenium ions (Ph-NH+) and phenyl oxenium ions (Ph-O+) have closed-shell singlet ground states with large singlet–triplet gaps resulting from a strong break in the degeneracy of the p orbitals on the formal nitrenium/oxenium center. Remarkably, we find computationally (CBS-QB3 and G4MP2) that azulenyl nitrenium and oxenium ions can have triplet ground states depending upon the attachment position on the azulene core. For instance, CBS-QB3 predicts that 1-azulenyl nitrenium ion and 1-azulenyl oxenium ion are singlet ground-state species with considerable singlet–triplet gaps of −47 and −45 kcal/mol to the lowest-energy triplet state, respectively. In contrast, 6-azulenyl nitrenium ion and 6-azulenyl oxenium ion have triplet ground states with a singlet–triplet gap of +7 and +10 kcal/mol, respectively. Moreover, the triplet states are π,π* states, rather than the typical n,π* states seen for many aryl nitrenium or oxenium ions. This dramatic switch in favored electronic states can be ascribed to changes in ring aromaticity/antiaromaticity, with the switch from ground-state singlet ions to triplet-favored ions resulting from both a destabilized singlet state (Hückel antiaromatic) and a stabilized triplet (Baird aromatic) state. Density functional theory (UB3LYP/6-31+G(d,p)) was used to determine substituent effects on the singlet–triplet energy gap for azulenyl nitrenium and oxenium ions, and we find that the unusual ground triplet states can be further tuned by employing electron-donating or -withdrawing groups on the azulene ring. This work demonstrates that azulenyl nitrenium and oxenium ions can have triplet π,π* ground states and provides a simple recipe for making ionic intermediates with distinct electronic configurations and consequent prediction of unique reactivity and magnetic properties from these species.

    Copyright © 2017 American Chemical Society

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    Supporting Information

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    The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.joc.7b02698.

    • Detailed coordinates and absolute energies for all compounds as well as additional LFER plots (PDF)

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    Cited By

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    This article is cited by 9 publications.

    1. Xin Ma, Ruth O. Anyaeche, Erlu Feng, Erynn Johnson, Ethan Roller, Daniel J. Rumley, John J. Nash, Hilkka I. Kenttämaa. Gas-Phase Reactivity of Quinoline-Based Singlet Oxenium Cations. The Journal of Organic Chemistry 2024, 89 (8) , 5458-5468. https://doi.org/10.1021/acs.joc.3c02895
    2. Yunfan Qiu, Lili Du, Sarah D. Cady, David Lee Phillips, Arthur H. Winter. Optical and EPR Detection of a Triplet Ground State Phenyl Nitrenium Ion. Journal of the American Chemical Society 2024, 146 (15) , 10679-10686. https://doi.org/10.1021/jacs.4c00511
    3. Ting Shen, Dandan Chen, Lu Lin, Jun Zhu. Dual Aromaticity in Both the T0 and S1 States: Osmapyridinium with Phosphonium Substituents. Journal of the American Chemical Society 2019, 141 (14) , 5720-5727. https://doi.org/10.1021/jacs.8b11564
    4. Daniel E. Falvey. Discrete Existence of Singlet Nitrenium Ions Revisited: Computational Studies of Non-Aryl Nitrenium Ions and Their Rearrangements. ACS Omega 2018, 3 (8) , 10418-10432. https://doi.org/10.1021/acsomega.8b01038
    5. Annunziata Soriente, Margherita De Rosa, Pellegrino La Manna, Carmen Talotta, Carmine Gaeta, Aldo Spinella, Placido Neri. Exploiting the p-Bromodienone Route for the Formation and Trapping of Calixarene Oxenium Cations with Enamine Nucleophiles. The Journal of Organic Chemistry 2018, 83 (11) , 5947-5953. https://doi.org/10.1021/acs.joc.8b00431
    6. Nabajyoti Patra, Astha Gupta, Prasad V. Bharatam. Stable, aromatic, and electrophilic azepinium ions: Design using quantum chemical methods. Journal of Computational Chemistry 2025, 46 (1) https://doi.org/10.1002/jcc.27520
    7. Wen Liu, Yonghui Tian. Observing C–N bond formation in plasma: a case study of benzene and dinitrogen coupling via an arylnitrenium ion intermediate. Physical Chemistry Chemical Physics 2024, 26 (26) , 18016-18020. https://doi.org/10.1039/D4CP01594K
    8. Lili Du, Juanjuan Wang, Yunfan Qiu, Runhui Liang, Penglin Lu, Xuebo Chen, David Lee Phillips, Arthur H. Winter. Generation and direct observation of a triplet arylnitrenium ion. Nature Communications 2022, 13 (1) https://doi.org/10.1038/s41467-022-31091-z
    9. Edward S. Chinn, Daniel E. Falvey. Photochemical generation and characterization of the 5-endo-10,11-dihydrodibenzoazepine nitrenium ion. Photochemical & Photobiological Sciences 2022, 21 (11) , 1907-1914. https://doi.org/10.1007/s43630-022-00267-3

    The Journal of Organic Chemistry

    Cite this: J. Org. Chem. 2017, 82, 24, 13550–13556
    Click to copy citationCitation copied!
    https://doi.org/10.1021/acs.joc.7b02698
    Published October 31, 2017
    Copyright © 2017 American Chemical Society

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