Synthesis and Spectroscopic Characterization of Hexakis(carbonyl)iron(II) Undecafluorodiantimonate(V), [Fe(CO)6][Sb2F11]2
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Abstract
Oxidative carbonylation of Fe(CO)5 in liquid SbF5 and a CO atmosphere, with either AsF5 or Cl2 as external oxidizing agents, produces [Fe(CO)6][Sb2F11]2 in very high yield. The resulting off-white solid material is thermally stable (above 200 °C). The homoleptic carbonyl cation [Fe(CO)6]2+, the first of its type formed by a 3d-metal, is isostructural with [Ru(CO)6]2+ and [Os(CO)6]2+ which are obtained by reductive carbonylation of M(SO3F)3, M = Ru or Os. The stretching force constant of 19.82 × 102 N m-1 and ν̄(CO)av of 2215.5 cm-1 suggest significantly reduced π-back-bonding. The single line 57Fe Mössbauer spectrum at δ = −0.001(6) mm s-1 relative to α-Fe is consistent with a regular octahedral structure and a 1A1g groundstate for [Fe(CO)6]2+. The possible existence of [Fe(CO)6]3+ formed by oxidation with Cl2 is discussed.
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