Synthesis of Chromium(IV) Nitrides Through High-Spin Tetrahedral Chromium(I) Intermediates

Panetti, Grace B.; Pecoraro, Matthew V.; Li, Runzi; Kim, Junho; Hierlmeier, Gabriele; Chirik, Paul J.

doi:10.1021/acs.inorgchem.5c05944

Synthesis of Chromium(IV) Nitrides Through High-Spin Tetrahedral Chromium(I) Intermediates

Journal Article · Thu Feb 19 00:00:00 EST 2026 · Inorganic Chemistry

DOI:https://doi.org/10.1021/acs.inorgchem.5c05944· OSTI ID:3022442

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Princeton University, NJ (United States)

Reduction of (depe)₂CrCl₂ (depe = 1,2-bis- (diethylphosphino)ethane) and (dep-benz)₂CrCl₂ (dep-benz = 1,2-bis(diethylphosphino)benzene) under 1 atm of N₂ furnished the dinitrogen complexes (depe)₂Cr(N₂)₂ and (dep-benz)₂Cr(N₂)₂, respectively. One-electron oxidation of these products with FcBAr^F ₄ (Fc = ferrocenium, BAr^F ₄ = B(3,5-(CF₃)₂C₆H₃)₄) yielded the unusual, high-spin tetrahedral complexes [(depe)₂Cr][BAr^F ₄] and [(dep-benz)₂Cr][BAr^F ₄] with concomitant loss of dinitrogen. Reaction of the chromium(I) derivatives with Ph₃CN₃ furnished rare examples of chromium(IV) nitrides as confirmed spectroscopically and by X-ray crystallography. While [(depe)₂Cr(≡N)][BAr^F ₄] underwent association of isocyanides accompanied by partial ligand dissociation, neither chromium nitride was reactive toward H₂ or diphenylsilane under thermal or photochemical conditions. These results distinguish the unique properties of the chromium(IV) nitrides as compared to heavier group 6 congeners and demonstrate both the feasibility of nitride synthesis and the limitations of dinitrogen cleavage and subsequent N−H bond formation.

View Accepted Manuscript (DOE)

Research Organization:: Princeton University, NJ (United States)

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

Grant/Contract Number:: SC0006498

OSTI ID:: 3022442

Journal Information:: Inorganic Chemistry, Journal Name: Inorganic Chemistry Journal Issue: 9 Vol. 65; ISSN 0020-1669; ISSN 1520-510X

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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