Inorganic metallocene derivatives containing only cyclo-P ligands have been targeted for more than 20 years, but their syntheses have never been achieved by pursuing the conventional route of using P phosphorus except for the generation of [Ti(η-P)]. Herein, we report a facile one-step method for the synthesis of the homoleptic iron complex [Fe(P)] by the Zintl-phase-type precursor KP. P NMR analyses indicate that upon dissolving the KP phase in ethylenediamine P was generated only in the presence of 2,2,2-crypt. The amounts of cation-sequestering agents, the type of iron precursor, and their consuming ratio have a decisive impact on the yield of [Fe(P)]. Both the Fe and the Fe precursors can oxidize P to give a concomitant product [(P)Fe(P)], which can be partially inhibited by the addition of potassium to produce relatively pure crystalline [K(2,2,2-crypt)][Fe(P)].
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