Intercalation of 2-aminoethylferrocene into the layered host lattices MoO3, 2H-TaS2and α-Zr(HPO4)2·H2O

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Abstract
The amino-functionalised ferrocene derivative FcCH2CH2NH2[Fc = Fe(η-C5H4)(η-C5H4)] has been intercalated under mild conditions into both single-crystal and microcrystalline samples of the layered host lattices MoO3, 2H-TaS2, and α-Zr(HPO4)2·H2O. The X-ray powder patterns for the new intercalates have been indexed and yield interlayer lattice expansions of 13.09, 5.89 and 14.54 Å, respectively. The large interlayer expansions of 13.09 and 14.5 Å observed for the intercalates of both MoO3 and α-Zr(HPO4)2·2H2O suggest the formation of a bilayer of guest molecules within these host lattices. The 57Fe Mössbauer spectrum of MoO3(FcCH2CH2NH2)0.36 exhibits a quadrupole doublet with an isomer shift δFe= 0.442 mm s–1 and quadrupole splitting Δ= 2.344 mm s–1, indicating the presence of unoxidised ferrocene molecules within the oxide layers. Solid-state 13C CP-MAS NMR spectra of MoO3(FcCH2CH2NH2)0.36 are consistent with the existence of both neutral FcCH2CH2NH2 and FcCH2CH2NH3 + moieties within the host. In addition, the changes in the electronic structure of MoO3 that accompany the interacalation of FcCH2CH2NH2 have been investigated by solid-state photoelectron spectroscopy.