Abstract
A new iron phosphate (NH 4) 4Fe 3(OH) 2F 2[H 3(PO 4) 4] has been synthesized hydrothermally at HF concentrations from 0.5 to 1.2 mL. Single-crystal X-ray diffraction analysis reveals its three-dimensional open-framework structure (monoclinic, space group P2 1 /n (No. 14), a=6.2614(13) Å, b=9.844(2) Å, c=14.271(3) Å, β=92.11(1)°, V=879.0(3) Å 3). This structure is built from isolated linear trimers of corner-sharing Fe(III) octahedra, which are linked by (PO 4) groups to form ten-membered-ring channels along [1 0 0]. This isolated, linear trimer of corner-sharing Fe(III) octahedra, [(FeO 4) 3(OH) 2F 2], is new and adds to the diverse linkages of Fe polyhedra as secondary building units in iron phosphates. The trivalent iron at octahedral sites for the title compound has been confirmed by synchrotron Fe K-edge XANES spectra and magnetic measurements. Magnetic measurements also show that this compound exhibit a strong antiferromagnetic exchange below T N=17 K, consistent with superexchange interactions expected for the linear trimer of ferric octahedra with the Fe–F–Fe angle of 132.5°.
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