A “Solvent‐Free” Crystal Structure of [Fe{N(SiMe ₃ ) ₂ } ₃ ] – Synthesis, Structure and Properties

For the synthesis of 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 which was isolated by sublimation product obtained reaction 2 eq FeCl3 with 3 LiN(SiMe3)2 in benzene. It could be characterized single crystal as well powder XRD and elemental analysis. However, 57Fe Mößbauer spectroscopy suggests contamination main an Fe(II) species. Also, part solid byproducts reactions solution were identified 7Li MAS NMR indicate distinct redox side between oxidizing reducing LiN(SiMe3)2, fact rationalizes lower than expected yields observation impurity compound. AC magnetic measurements have been performed extended frequency range up to 104 s−1, allowing for more precise evaluation relaxation parameters when compared previously published measurements.