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A “Solvent-Free” Crystal Structure of [FeN(SiMe3)23] – Synthesis, Structure and Properties

Indris, Sylvio; Knapp, Michael; Schwarz, Björn; Eichhöfer, Andreas

Abstract:
For the synthesis of the ferric bis(trimethylsilyl)amido complex [Fe{N(SiMe3)2}3] literature gives differing synthetic protocols based on crystallization from solution. In this report we present a ‘solvent‐free’ structural phase of [Fe{N(SiMe$_{3}$)$_{2}$}$_{3}$] which was isolated by sublimation of the product obtained from the reaction of 2 eq FeCl$_{3}$ with 3 eq LiN(SiMe$_{3}$)$_{2}$ in benzene. It could be characterized by single crystal as well as powder XRD and elemental analysis. However, $_{57}$Fe Mößbauer spectroscopy suggests a contamination of the main product with an Fe(II) species. Also, a part of the solid reaction byproducts from the reactions in solution were identified by powder XRD and $_{7}$Li MAS NMR which indicate distinct redox side reactions between oxidizing FeCl$_{3}$ and reducing LiN(SiMe$_{3}$)$_{2}$, a fact which rationalizes the lower than expected yields and the observation of an Fe(II) impurity compound. AC magnetic measurements of [Fe{N(SiMe$_{3}$)$_{2}$}$_{3}$] ave been performed in an extended frequency range up to 10$^{4}$ s$^{-1}$ allowing for a more precise evaluation of the magnetic relaxation parameters when compared to previously published measurements.

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Verlagsausgabe §
DOI: 10.5445/IR/1000130335
Veröffentlicht am 10.03.2021
Cover der Publikation
Zugehörige Institution(en) am KIT Institut für Angewandte Materialien - Energiespeichersysteme (IAM-ESS)
Publikationstyp Zeitschriftenaufsatz
Publikationsjahr 2021
Sprache Englisch
Identifikator ISSN: 1434-1948, 0009-2940, 0365-947X, 0365-9488, 0365-9496, 1099-0682, 1434-2421
KITopen-ID: 1000130335
Erschienen in European Journal of Inorganic Chemistry
Verlag Wiley-VCH Verlag
Band 2021
Heft 10
Seiten 951-959
Schlagwörter iron; amides; Fe-Mößbauer spectroscopy; Li-NMR spectroscopy; magnetic properties
Nachgewiesen in Scopus
Web of Science
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