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An Intermediate Cobalt(IV) Nitrido Complex and its N-Migratory Insertion Product

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‡ Department of Chemistry and Pharmacy, Inorganic Chemistry, Friedrich-Alexander University Erlangen - Nürnberg (FAU), Egerlandstr. 1, 91058 Erlangen, Germany
∥ Université de Toulouse et CNRS, NSA, UPS, CNRS, UMR 5215 LPCNO, 135 avenue de Rangueil, 31077 Toulouse, France
§ Max Planck Institute for Chemical Energy Conversion, Stiftstraße 34−36, 45470 Mülheim, Germany
[email protected]
Cite this: J. Am. Chem. Soc. 2014, 136, 42, 15072–15078
Publication Date (Web):September 22, 2014
https://doi.org/10.1021/ja508144j
Copyright © 2014 American Chemical Society
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    Low-temperature photolysis experiments (T = 10 K) on the tripodal azido complex [(BIMPNMes,Ad,Me)CoII(N3)] (1) were monitored by EPR spectroscopy and support the formation of an exceedingly reactive, high-valent Co nitrido species [(BIMPNMes,Ad,Me)CoIV(N)] (2). Density functional theory calculations suggest a low-spin d5, S = 1/2, electronic configuration of the central cobalt ion in 2 and, thus, are in line with the formulation of complex 2 as a genuine, low-spin Co(IV) nitride species. Although the reactivity of this species precludes handling above 50 K or isolation in the solid state, the N-migratory insertion product [(NH-BIMPNMes,Ad,Me)CoII](BPh4) (3) is isolable and was reproducibly synthesized as well as fully characterized, including CHN elemental analysis, paramagnetic 1H NMR, IR, UV–vis, and EPR spectroscopy as well as SQUID magnetization and single-crystal X-ray crystallography studies. A computational analysis of the reaction pathway 2 → 3 indicates that the reaction readily occurs via N-migratory insertion into the Co–C bond (activation barrier of 2.2 kcal mol–1). In addition to the unusual reactivity of the nitride 2, the resulting divalent cobalt complex 3 is a rare example of a trigonal pyramidal complex with four different donor ligands of a tetradentate chelate—an N-heterocyclic carbene, a phenolate, an imine, and an amine—binding to a high-spin Co(II) ion. This renders complex 3 chiral-at-metal.

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