Nitrogen-15 and Carbon-13 NMR Study of Roussin Salts and Esters and of Pentacyanoferrate Complexes

Anthony R. Butler, Christopher Glidewell, Andrew R. Hyde, Joseph Mcginnis

    Research output: Contribution to journalArticle

    49 Citations (Scopus)

    Abstract

    High-frequency 15N NMR spectroscopy, using 99% isotopic enrichment for 15N, shows that the Roussin esters Fe2(SR)2(NO)4 (R = Me, i'-Pr) exist as an equimolar mixture of two conformers having and C2v symmetries respectively. Similar 15N spectroscopy of [Fe4X3(NO)7]- (X = S, Se) shows that the solid-state structure for X = S persists in aqueous solution and demonstrates that the anion having X = Se is isostructural in solution; this is confirmed by natural-abundance 77Se NMR. The cubane type Fe4S4(NO)4 retains its structure in solution, and Fe4Se4(NO)4 is isostructural. A combination of 13C and 15N NMR spectra obtained at high frequency with 90% 13C and 99% 15N enrichment reveals two mechanisms for the conversion of [Fe-(CN)5NO]2- to [Fe(CN)5N02]4-, one involving nucleophilic attack by hydroxide and the other attack by nitrite. The spectral data allow ready identification of pentacyanoferrate complexes arising from the reactions of nitroprusside with nucleophiles.

    Original languageEnglish
    Pages (from-to)2931-2934
    Number of pages4
    JournalInorganic Chemistry
    Volume24
    Issue number19
    DOIs
    Publication statusPublished - 1 Sep 1985

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