Tale of Three Molecular Nitrides: Mononuclear Vanadium (V) and (IV) Nitrides As Well As a Mixed-Valence Trivanadium Nitride Having a V3N4 Double-Diamond Core

Jafari, Mehrafshan G.; Fehn, Dominik; Reinholdt, Anders; Hernández-Prieto, Cristina; Patel, Prajay; Gau, Michael R.; Carroll, Patrick J.; Krzystek, J.; Liu, Cong; Ozarowski, Andrew; Telser, Joshua; Delferro, Massimiliano; Meyer, Karsten; Mindiola, Daniel J.

doi:10.1021/jacs.2c00276

Tale of Three Molecular Nitrides: Mononuclear Vanadium (V) and (IV) Nitrides As Well As a Mixed-Valence Trivanadium Nitride Having a V₃N₄ Double-Diamond Core

Journal Article · Thu Jun 02 00:00:00 EDT 2022 · Journal of the American Chemical Society

DOI:https://doi.org/10.1021/jacs.2c00276· OSTI ID:1923254

^[1]; Fehn, Dominik ^[2]; ^[1]; Hernández-Prieto, Cristina ^[1]; ^[3]; ^[1]; ^[1]; ^[4]; ^[3]; ^[4]; ^[5]; ^[6]; ^[2]; ^[1]

Univ. of Pennsylvania, Philadelphia, PA (United States)
Friedrich-Alexander-University Erlangen-Nürnberg (FAU) (Germany)
Argonne National Lab. (ANL), Argonne, IL (United States)
Florida State Univ., Tallahassee, FL (United States). National High Magnetic Field Lab. (MagLab)
Roosevelt University, Chicago, IL (United States)
Argonne National Lab. (ANL), Lemont, IL (United States)

Here, transmetallation of [VCl₃(THF)₃] and [TlTp^tBu,Me] afforded [(Tp^tBu,Me)VCl₂] (1, Tp^tBu,Me = hydro-tris(3-tert-butyl-5-methylpyrazol-1-yl)borate), which was reduced with KC₈ to form a $$C_{3v}$$ symmetric V^II complex, [(Tp^tBu,Me)VCl] (2). Complex 1 has a high-spin ($$\textit{S}$$ = 1) ground state and displays rhombic high-frequency and -field electron paramagnetic resonance (HFEPR) spectra, while complex 2 has an $$\textit{S}$$ = 3/2 ⁴A₂ ground state observable by conventional EPR spectroscopy. Complex 1 reacts with NaN₃ to form the V^V nitride-azide complex [(Tp^tBu,Me)V≡N(N₃)] (3). A likely V^III azide intermediate en route to 3, [(Tp^tBu,Me)VCl(N₃)] (4), was isolated by reacting 1 with N₃SiMe₃. Complex 4 is thermally stable but reacts with NaN3 to form 3, implying a bis-azide intermediate, [(Tp^tBu,Me)V(N₃)₂] (A), leading to 3. Reduction of 3 with KC₈ furnishes a trinuclear and mixed-valent nitride, [{(Tp^tBu,Me)V}₂($$μ_{4-}$$VN₄)] (5), conforming to a Robin–Day class I description. Complex 5 features a central vanadium ion supported only by bridging nitride ligands. Contrary to 1, complex 2 reacts with NaN₃ to produce an azide-bridged dimer, [{(Tp^tBu,Me)V}₂(1,3-$$μ_2$$-N₃)₂] (6), with two antiferromagnetically coupled high-spin V^II ions. Complex 5 could be independently produced along with [($$κ_2$$-Tp^tBu,Me)₂V] upon photolysis of 6 in arene solvents. The putative {V^IV≡N} intermediate, [(Tp^tBu,Me)V≡N] (B), was intercepted by photolyzing 6 in a coordinating solvent, such as tetrahydrofuran (THF), yielding [(Tp^tBu,Me)V≡N(THF)] (B-THF). In arene solvents, B-THF expels THF to afford 5 and [($$κ_2$$-Tp^tBu,Me)₂V]. A more stable adduct (B-OPPh₃) was prepared by reacting B-THF with OPPh₃. These adducts of B are the first neutral and mononuclear V^IV nitride complexes to be isolated.

View Accepted Manuscript (DOE)

Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States). Laboratory Computing Resource Center (LCRC)

Sponsoring Organization:: Carlsberg Foundation; Independent Research Fund Denmark; National Institutes of Health (NIH); National Science Foundation (NSF); State of Florida; USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division; University of Pennsylvania

Grant/Contract Number:: AC02-06CH11357; SC0019342

OSTI ID:: 1923254

Journal Information:: Journal of the American Chemical Society, Journal Name: Journal of the American Chemical Society Journal Issue: 23 Vol. 144; ISSN 0002-7863

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Synthesis, structure and reactivity of a terminal magnesium fluoride compound, [Tp ^But,Me ]MgF: hydrogen bonding, halogen bonding and C–F bond formation Rauch, Michael; Ruccolo, Serge; Mester, John Paul Chemical Science, Vol. 7, Issue 1 https://doi.org/10.1039/c5sc03504j	journal	January 2016
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Tale of Three Molecular Nitrides: Mononuclear Vanadium (V) and (IV) Nitrides As Well As a Mixed-Valence Trivanadium Nitride Having a V3N4 Double-Diamond Core

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