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Montclare, Jin
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article
Structural and <sup>1</sup>H NMR spectroscopic characterization of bis(N-isopropylsalicylaldiminato)iron(II)
Abstract
<p>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 (L<sup>ipr</sup>H) 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(O<sub>2</sub>CCH<sub>3</sub>)<sub>2</sub> in KOH-CH<sub>3</sub>OH to produce a precursor formulated as Fe(sal)<sub>2</sub> which is reacted subsequently with isopropylamine in THF to form Fe(L<sup>ipr</sup>)<sub>2</sub> in 34% isolated yield. A single crystal X-ray crystallographic study of Fe(L<sup>ipr</sup>)<sub>2</sub> reveals a mononuclear complex with two bidentate salicylaldiminate ligands bound to an iron(II) atom in a tetrahedral coordination geometry. The <sup>1</sup>H NMR spectrum of Fe(L<sup>ipr</sup>)<sub>2</sub> in benzene-d<sub>6</sub> 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(L<sup>ipr</sup>)<sub>2</sub> forms the oxo-bridged dinuclear iron(III) complex [(L<sup>ipr</sup>)<sub>2</sub>Fe]<sub>2</sub>O as shown by <sup>1</sup>H NMR spectroscopy. © 2002 Elsevier Science Ltd. All rights reserved.</p>