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Un complejo intermedio de nitruro de cobalto (IV) y su producto de inserción N-migrante
Eva M Zolnhofer1, Martina Käß, Marat M Khusniyarov
1Department of Chemistry and Pharmacy, Inorganic Chemistry, Friedrich-Alexander University Erlangen - Nürnberg (FAU) , Egerlandstr. 1, 91058 Erlangen, Germany.
Journal of the American Chemical Society
|September 23, 2014
Resumen
Los experimentos a baja temperatura revelan una especie de nitruro de cobalto (IV) altamente reactivo formado a partir de un complejo de azido. Este nitruro transitorio se somete a una inserción N-migrante, dando como resultado un raro complejo quiral, trigonal y piramidal de cobalto (II).
Área de la Ciencia:
- Química Inorgánica La Química Inorgánica es la química inorgánica.
- Química organometálica Química orgánica de los metales.
- La espectroscopia es una técnica de espectroscopia.
Sus antecedentes:
- Investigar la reactividad de las especies de nitruro metálico de baja coordinación y alta valencia es crucial para comprender los mecanismos de transferencia de nitrógeno.
- Los complejos de azido sirven como precursores para generar nitrido reactivo intermedio.
- La configuración electrónica y el estado de giro de los centros metálicos dictan su reactividad y estabilidad.
Objetivo del estudio:
- Para sintetizar y caracterizar una especie de nitruro de cobalto de alta valencia.
- Para dilucidar la vía de reacción del intermediario del nitruro de cobalto.
- Caracterizar el producto de inserción migratoria N resultante y sus características estructurales únicas.
Principales métodos:
- Fotólisis a baja temperatura (10 K) de un complejo de azido cobalto.
- Espectroscopia de resonancia paramagnética de electrones (EPR) para el monitoreo intermedio.
- Cálculos de la Teoría Funcional de Densidad (DFT) para la estructura electrónica y las vías de reacción.
- Caracterización completa del producto utilizando análisis elemental CHN, RMN, IR, UV-vis, magnetometría SQUID y cristalografía de rayos X. Caracterización completa del producto utilizando análisis elemental CHN, RMN, IR, UV-vis, magnetometría SQUID y cristalografía de rayos X. Caracterización completa del producto utilizando análisis elemental CHN, NMR, IR, UV-vis, magnetometría SQUID y cristalografía de rayos X. Caracterización completa del producto utilizando análisis elemental CHN, NMR, IR, UV-vis, magnetometría SQUID y cristalografía de rayos X.
Principales resultados:
- Formación de una especie de nitruro de cobalto (IV) altamente reactivo y de alta valencia (2) a partir del precursor de azido (1) a bajas temperaturas.
- Los cálculos de DFT apoyan una configuración de bajo espín d(5), S=1/2 para el nitruro de cobalto.
- Aislamiento y caracterización del producto de inserción N-migrante, un complejo trigonal piramidal de cobalto (II) (3).
- La vía de reacción desde el nitruro (2) hasta el producto (3) procede a través de una inserción N-migrante fácil con una barrera de activación baja (2,2 kcal mol(-1)).
Conclusiones:
- El estudio demuestra la generación y caracterización de una especie transitoria de nitruro de cobalto (IV) de alta valencia.
- El nitruro de cobalto (IV) se somete a una fácil inserción migratoria de N en un enlace Co-C.
- El complejo de cobalto (II) resultante (3) es un raro ejemplo de un complejo piramidal quiral y trigonal con diversos ligandos donantes, destacando una química de coordinación inusual.
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