Hydrothermal Synthesis, Structure, and Magnetic Properties of a Layered Fe(III) Carboxymethylphosphonate: [Fe(H2O)(O3P–CH2–CO2)] or MIL-49

Author： Sanselme M.   Riou-Cavellec M.   Grenèche J-M.   Férey G.  

Publisher： Academic Press

ISSN： 0022-4596

Source： Journal of Solid State Chemistry, Vol.164, Iss.2, 2002-03, pp. : 354-360

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Abstract

[FeIII(H2O)(O3P– (CH2)–CO2)] or MIL-49 was hydrothermally synthesized under autogenous pressure at 170°C for 48 h. Its bidimensional structure was solved from single-crystal X-ray diffraction in the monoclinic space group P21/c (No.14). Cell parameters are a =9.3836(3) Å, b=6.3798(3) Å, c=10.1371(3) Å, β=111.891(2)°, Z=4, and V=563.10(4) Å3. Reliability factors of the structure refinement are R1(F)=0.0470 and wR2(F2)=0.1297 for 1036 reflections with I>2σ(I). The structure of MIL-49 is based on inorganic units built up from two edge-sharing [FeO5(H2O)] octahedra and two carboxymethylphosphonate groups. The connection of these units leads to the formation of hybrid sheets. A dangling oxygen atom from the carboxy function points toward the interlayer space and is responsible for hydrogen bonding with adjacent layers. Magnetic measurements and 57Fe Mössbauer study reveal an antiferromagnetic ordering below TN=25(1) K which becomes canted below 11(1) K. © 2002 Elsevier Science (USA).

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