Synthesis, crystal structure, magnetic susceptibility, and Mössbauer spectroscopy of a mixed-valence organic-inorganic hybrid compound: (H3DETA)[Fe3(C2O4) 2(HPO4)2(PO4)] (DETA = diethylenetriamine)

Yau Chen Jiang, Sue Lein Wang, Kwang Hwa Lii, Ninh Nguyen, Annie Ducouret

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Abstract

A mixed-valence organic-inorganic hybrid compound, (H3DETA) [Fe3(C2O4)2 (HPO4)2(PO4)] (DETA = diethylenetriamine), has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, magnetic susceptibility, 57Fe powder absorption Mössbauer spectroscopy, and electric field gradient calculations. It crystallizes in the triclinic space group P1 (No. 2) with a = 9.6367(7) Å, b = 10.1760(7) Å, c = 12.6164(9) Å, α = 86.302(1)°, β = 68.880(1)°, γ = 61.800(1)°, and Z = 2 with R1 = 0.0397. The structure can be described as layers of trigonal bipyramidal FeIIO5, octahedral FeIIIO6, tetrahedral PO4 moieties, and monobidentate oxalate ligands, which are pillared through bisbidentate oxalate ligands to form a 3-D framework structure. The title compound is not only the first oxalatophosphate that contains two types of oxalate ligands but also the first example of mixed-valence transition metal oxalatophosphate.

Original languageEnglish
Pages (from-to)1633-1638
Number of pages6
JournalChemistry of Materials
Volume15
Issue number8
DOIs
StatePublished - 22 Apr 2003

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