Hydrothermal synthesis and structural characterization of a gallium pyromellitate Ga(OH)(btec)•0.5H2O, with infinite Ga-(μ2-OH)Ga chains (MIL-61)

被引:43
作者
Loiseau, T [1 ]
Muguerra, H [1 ]
Haouas, M [1 ]
Taulelle, F [1 ]
Férey, G [1 ]
机构
[1] Univ Versailles, Inst Lavoisier, CNRS, UMR 8637, F-78035 Versailles, France
关键词
hydrothermal synthesis; gallium; 1,2,4,5-benzenetetracarboxylic acid; metal-organic frameworks; X-ray powder diffraction; solid state NMR; H-1; C-13;
D O I
10.1016/j.solidstatesciences.2005.01.014
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
A new gallium carboxylate Ga(OH)(btec)center dot 0.5H(2)O (MIL-61) was synthesized under mild hydrothermal conditions (200 degrees C, 24 hours) in the presence of 1,2,4,5-benzenetetracarboxylic (btec) acid and water. The crystal structure, characterized by means of Rietevelt refinement of powder XRD data, consists of trans chains of GaO4(OH)(2) octahedra, connected to each other through a mu(2)-OH group. The three-dimensional framework is built up from these chains linked together via the organic molecules so delimiting the cavities where the water molecules are encapsulated. Analysis by solid state NMR (1 H and C-13) has confirmed the presence within the structure of both water molecules and carboxylate moieties partially deprotonated. The structure of Ga(OH)(btec)center dot 0.5H(2)O corresponds to that of MIL-61 obtained with vanadium replacing gallium. Crystal data for Ga-4(OH)(4)((HO2C)(2)-C6H4-(CO2)(2))(4)center dot 2H(2)O: a = 14.8325(10) angstrom, b = 6.7792(10) angstrom, c = 10.6726(10) angstrom, V 1073.2(2) angstrom(3), Prima (n degrees 62). (c) 2005 Elsevier SAS. All rights reserved.
引用
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页码:603 / 609
页数:7
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