Research in our lab has led to the synthesis of imide and imide-sulfide cubane-like clusters with general formula [Fe4(NtBu)nS4-nCl4]z (n = 1-4). This series connects at n = 0 which is the previously known, well studied all-sulfide cluster. The other terminal member, the n = 4 all-imide cluster, has been only briefly reported by ourselves and the laboratory of Fenske. Continuing studies in the chemistry of this cluster series have prompted us to reinvestigate the chemistry of the all-imide cluster. The synthesis of [Fe4(NtBu)4Cl4]1- involves the simple reaction of FeCl3 and two equivalents of LiNHtBu. Different reaction outcomes and quantities of [Fe4(NtBu)4Cl4]1- arise from changes in reaction conditions. A ubiquitous by-product in the reaction chemistry is FeCl2(NH2tBu)2 which contains amine ligands that undergo chemical exchange on the NMR timescale. We report here the study of reaction conditions that lead to the formation of the all-imide cluster, the equilibrium solution study of FeCl2(NH2tBu)2 and the structural and physical characterization of the redox series [Fe4(NtBu)4Cl4]0, 1-, 2-.

Further investigation of the synthesis and properties of iron-imide clusters

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ACS Fall 2022

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