Structural and 1H NMR spectroscopic characterization of bis(N-isopropylsalicylaldiminato)iron(II)

Michele A. Torzilli, Shalton Colquhoun, Jin Montclare, Robert H. Beer

Research output: Contribution to journalArticle

Abstract

Coordinatively unsaturated iron(II) species form reactive organometallic and coordination complexes and are integral to the reactivity of non-heme iron proteins and their synthetic analogues. Iron(II) Schiff base complexes have proven to be easily prepared and useful starting materials for such compounds. Here we report a detailed preparative procedure and the solid-state structure of the iron(II) complex of N-isopropylsalicylaldimine (LiprH) based on the compounds first synthesized by Larkworthy (J. Chem. Soc., A (1968) 1048). The title compound is prepared by adding 2 equiv. of salicylaldehyde (sa1H) to Fe(O2CCH3)2 in KOH-CH3OH to produce a precursor formulated as Fe(sal)2 which is reacted subsequently with isopropylamine in THF to form Fe(Lipr)2 in 34% isolated yield. A single crystal X-ray crystallographic study of Fe(Lipr)2 reveals a mononuclear complex with two bidentate salicylaldiminate ligands bound to an iron(II) atom in a tetrahedral coordination geometry. The 1H NMR spectrum of Fe(Lipr)2 in benzene-d6 exhibits six paramagnetically shifted ligand resonances ranging from +195 to -31 ppm that are consistent with a mononuclear high spin (S = 2) iron(II) complex in solution. Upon exposure to air, Fe(Lipr)2 forms the oxo-bridged dinuclear iron(III) complex [(Lipr)2Fe]2O as shown by 1H NMR spectroscopy.

Original languageEnglish (US)
Pages (from-to)705-713
Number of pages9
JournalPolyhedron
Volume21
Issue number7
DOIs
StatePublished - Apr 1 2002

Keywords

  • H NMR spectroscopy
  • Dioxygen reactivity
  • Iron(II)
  • Schiff base
  • X-ray crystal structures
  • Zinc(II)

ASJC Scopus subject areas

  • Biochemistry
  • Inorganic Chemistry
  • Physical and Theoretical Chemistry
  • Materials Chemistry

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