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Hydrothermal syntheses and crystal structures of two new iron phosphates [C2N2H10]2+[Fe(HPO4)2(OH)]2-.H2O and KFe3(OH)2(PO4)2.2H2O

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ZAD Lethbridge, Philip Lightfoot, Russell Edward Morris, DS Wragg, Paul Anthony Wright, Å Kvick, G Vaughan

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Two new iron phosphates have been prepared hydrothermally and characterized by single crystal X-ray diffraction. [C2N2H10](2+) [Fe(HPO4)(2)(OH)](2-) . H2O (I) crystallizes in tri-clinic space group P-1, a = 8.526(2) Angstrom, b = 9.796(2) Angstrom, c = 7.232(2) Angstrom, alpha = 90.25(2)degrees, beta = 92.72(2)degrees, gamma = 65.20(1)degrees, Z = 2, R, R-w = 0.040, 0.044. The structure is composed of isolated anionic chains of the tancoite type, [Fe(HPO4)(2)OH](n), consisting of vertex-sharing Fe-O octahedra, The chains are isotypic with those in the iron fluorophosphate ULM-14, but in that case the vertex-sharing is via an F- link rather than an OH- link, KFe3(OH)(2)(PO4)(2) . 2H(2)O (II) adopts the orthorhombic space group Pmc2(1), a = 6.410(2) Angstrom, b = 7.329(3) Angstrom, c = 9.868(4) Angstrom, Z = 2, R, R-w = 0.053, 0.090. In this case the structure was solved from microcrystal diffraction data at a synchrotron source (crystal size 60 x 15 x 5 pm), The structure is isotypic with the mineral olmsteadite, KFe2NbO2(PO4)(2) . 2H(2)O, with Fe3+ on the Nb5+ site and charge-balancing OH- groups replacing O2-. This compound has a three-dimensional framework structure with small channels running parallel to a and c in which the K+ ions sit, (C) 1999 Academic Press.



Original languageEnglish
Pages (from-to)455-460
Number of pages6
JournalJournal of Solid State Chemistry
Publication statusPublished - 1 Feb 1999

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