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

Indris, Sylvio 1; Knapp, Michael 1; Schwarz, Björn 1; Eichhöfer, Andreas 2
1 Institut für Angewandte Materialien – Energiespeichersysteme (IAM-ESS), Karlsruher Institut für Technologie (KIT)
2 Institut für Nanotechnologie (INT), Karlsruher Institut für Technologie (KIT)

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.


Verlagsausgabe §
DOI: 10.5445/IR/1000130335
Veröffentlicht am 10.03.2021
Originalveröffentlichung
DOI: 10.1002/ejic.202001055
Scopus
Zitationen: 2
Web of Science
Zitationen: 2
Dimensions
Zitationen: 2
Cover der Publikation
Zugehörige Institution(en) am KIT Institut für Angewandte Materialien – Energiespeichersysteme (IAM-ESS)
Institut für Nanotechnologie (INT)
Publikationstyp Zeitschriftenaufsatz
Publikationsdatum 12.03.2021
Sprache Englisch
Identifikator ISSN: 1434-1948, 0009-2940, 0365-947X, 0365-9488, 0365-9496, 1099-0682, 1434-2421
KITopen-ID: 1000130335
HGF-Programm 38.02.01 (POF IV, LK 01) Fundamentals and Materials
Erschienen in European Journal of Inorganic Chemistry
Verlag Wiley-VCH Verlag
Band 2021
Heft 10
Seiten 951-959
Vorab online veröffentlicht am 16.02.2021
Schlagwörter iron, amides, Fe-Mößbauer spectroscopy, Li-NMR spectroscopy, magnetic properties; 2015-015-008770 SCXD
Nachgewiesen in Dimensions
Web of Science
Scopus
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