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2007
ACL
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C.Volkringer, T.Loiseau, G.Férey, C.M.Morais, F.Taulelle, V.Montouillout, D.Massiot, 'Synthesis, crystal structure and 71Ga solid state NMR of a MOF-type gallium trimesate (MIL-96) with µ3-oxo bridged trinuclear units and a hexagonal 18-ring network', Microporous Mesoporous Mat. 105 111-117 (2007) doi:10.1016/j.micromeso.2007.05.018
A new gallium trimesate Ga12O(OH)12({OH}4,{H2O}5)[btc]6 24H2O, called MIL-96, (btc = 1,3,5- benzenetricarboxylate or trimesate species) was hydrothermally synthesized under mild conditions (210 C, 5 h) in the presence of trimethyl 1,3,5-benzenetricarboxylate in water and characterized by single-crystal X-ray diffraction technique. The MIL-96 (Ga) structure exhibits a three-dimensional metal– organic framework containing isolated trinuclear l3-oxo-bridged gallium clusters and infinite chains of GaO4(OH)2 and GaO2(OH)4 octahedra generating a hexagonal network based on 18-membered ring. The two types of gallium groups are connected to each other through the trimesate species which induce corrugated chains of gallium octahedra, linked via l2-hydroxo bonds with the specific -cis–cis–trans- sequence. The 3D framework of MIL-96 reveals three kinds of cavities (two of them have estimated pore volumes of 480 and 860 A˚ 3), in which are encapsulated free water molecules. The latter species are removed upon heating at 150 C. The MIL- 96 (Ga) compound was characterized by 71Ga solid state NMR at different magnetic fields (14.1 and 17.6 T). 71Ga spectra of MIL-96 (Ga) show the gallium exhibits relatively weak quadrupolar interactions compared to those observed in other MOF-type gallium carboxylates that have very strong quadrupolar interactions (MIL-61 and MIL-53).
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