Hydrothermal Synthesis, Structure, and Solid State 19 F NMR Study of ULM-17: (H 3 O) 2 [V 4 (HPO 4 )(PO 4 ) 3 O 6 F] 2 [NC 7 H 14 ] 6
1996; American Chemical Society; Volume: 35; Issue: 22 Linguagem: Inglês
10.1021/ic960081t
ISSN1520-510X
AutoresD. Riou, Françis Taulelle, Gérard Férey,
Tópico(s)Crystal Structures and Properties
Resumo(H3O)2[V4(HPO4)(PO4)3O6F]2[NC7H14]6 (labeled ULM-17) has been hydrothermally synthesized (150°, 24 h, autogeneous pressure). It is monoclinic (space group P21/c (No. 14)) with a = 21.4747(6) Å, b = 17.7223(5) Å, c = 20.1616(6) Å, β = 94.329(1)°, and Z = 4. The structure consists in the hexagonal close packing of discrete hydronium cations, protonated quinuclidine and molecular anions [V4(HPO4)(PO4)3O6F]4- (1) The structure presents two kinds of octameric anions built up from the tetrahedral arrangement of VVO5F octahedra sharing edges and vertices, capped by phosphorus tetrahedra. The stability of the solid is ensured via strong hydrogen bonds between the oxygens of the polyanions and the hydrogens of both hydronium and quinuclidinium cations. The particuliar location of fluorine at the center of the molecular anion 4-fold coordinated by VV was studied by solid state NMR.
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