TY - JOUR
T1 - The first organically templated layered iron phosphate
T2 - Hydrothermal synthesis, structure, magnetic properties, and the Mössbauer spectrum of [H3NCH2CH2NH3] 0.5[Fe(OH)(PO4)]
AU - DeBord, Jeffrey R.D.
AU - Reiff, William M.
AU - Haushalter, Robert C.
AU - Zubieta, Jon
N1 - Funding Information:
The work at Syracuse University was supported by NSF Grant CHE-9318824. J.Z. also acknowledges the donors of the Petroleum Research Fund, administered by the American Chemical Society, for support of the research at Syracuse under Grant PRF 30651-AC5, 3. W.M.R. acknowledges the NSF Division of Materials Research for funds for the ac susceptometer.
PY - 1996/9/5
Y1 - 1996/9/5
N2 - The first organically templated, layered iron phosphate [H3NCH2CH2NH3] 0.5[Fe(OH)(PO4)], 1, has been prepared and characterized via single crystal X-ray diffraction, variable temperature magnetic susceptibility measurements, and Mössbauer spectroscopy. Phosphate 1 is synthesized from the hydrothermal reaction of FeCl3, H3PO4, ethylenediamine, and H2O in the mole ratio 1:3.6:4.2:444 for 64 h at 160°C and exhibits a layered structure consisting of infinite chains of edge-sharing {FeO6} octahedra linked into finite 2-D sheets by {PO4} tetrahedra that possess terminal P=O groups which protrude into the interlamellar space. The infinite edge-sharing chains display a pairwise puckering resulting from the presence of trans μ2-OH groups arranged in a zig-zag fashion along the chain. The charge compensating ethylenediammonium cations contact both adjacent layers via an elaborate and complicated hydrogen bonded network. Crystal data for 1: FePO5NCH6, monoclinic, space group P21/c, a = 4.5010(7) Å, b = 6.114(1) Å, c = 18.460(3) Å, β = 94.59(1)°, V = 56.4(1) Å, Z = 2, dcalc = 2.608 g · cm-3; 1650 reflections, R = 0.049. Variable temperature Mossbauer data, dc magnetization, and ac susceptibility measurements show that 1 undergoes a transition to a weak ferromagnetic State near 30 K.
AB - The first organically templated, layered iron phosphate [H3NCH2CH2NH3] 0.5[Fe(OH)(PO4)], 1, has been prepared and characterized via single crystal X-ray diffraction, variable temperature magnetic susceptibility measurements, and Mössbauer spectroscopy. Phosphate 1 is synthesized from the hydrothermal reaction of FeCl3, H3PO4, ethylenediamine, and H2O in the mole ratio 1:3.6:4.2:444 for 64 h at 160°C and exhibits a layered structure consisting of infinite chains of edge-sharing {FeO6} octahedra linked into finite 2-D sheets by {PO4} tetrahedra that possess terminal P=O groups which protrude into the interlamellar space. The infinite edge-sharing chains display a pairwise puckering resulting from the presence of trans μ2-OH groups arranged in a zig-zag fashion along the chain. The charge compensating ethylenediammonium cations contact both adjacent layers via an elaborate and complicated hydrogen bonded network. Crystal data for 1: FePO5NCH6, monoclinic, space group P21/c, a = 4.5010(7) Å, b = 6.114(1) Å, c = 18.460(3) Å, β = 94.59(1)°, V = 56.4(1) Å, Z = 2, dcalc = 2.608 g · cm-3; 1650 reflections, R = 0.049. Variable temperature Mossbauer data, dc magnetization, and ac susceptibility measurements show that 1 undergoes a transition to a weak ferromagnetic State near 30 K.
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U2 - 10.1006/jssc.1996.0284
DO - 10.1006/jssc.1996.0284
M3 - Article
AN - SCOPUS:0000518454
SN - 0022-4596
VL - 125
SP - 186
EP - 191
JO - Journal of Solid State Chemistry
JF - Journal of Solid State Chemistry
IS - 2
ER -