CRYSTAL-STRUCTURE AND SOLID-STATE NUCLEAR-MAGNETIC-RESONANCE CHARACTERIZATION OF AN OXYFLUORINATED 3-DIMENSIONAL FRAMEWORK GALLOPHOSPHATE WITH ULM-4 STRUCTURAL TYPE - STRUCTURAL RELATIONSHIPS WITH GAASO4-2
T. Loiseau et al., CRYSTAL-STRUCTURE AND SOLID-STATE NUCLEAR-MAGNETIC-RESONANCE CHARACTERIZATION OF AN OXYFLUORINATED 3-DIMENSIONAL FRAMEWORK GALLOPHOSPHATE WITH ULM-4 STRUCTURAL TYPE - STRUCTURAL RELATIONSHIPS WITH GAASO4-2, Microporous materials, 9(1-2), 1997, pp. 83-93
Ga-3(PO4)(3)F-2, 0.75 H3N(CH2)(3)NH3, 0.5 H3O (ULM-4) was obtained by
hydrothermal synthesis (453 K, 24 h, autogenous pressure) from a mixtu
re of Ga2O3, H3PO4, HF, 1,3-diaminopropane and H2O in the ratio 1:2:2:
1.3:80. The structure was studied by single-crystal X-ray diffraction
and solid state NMR. It is monoclinic (space group P2(1)/n (no. 14)) w
ith a = 8.674(1) Angstrom, b = 10.190(2) Angstrom, c=16.826(3) Angstro
m, beta = 94.21(2)degrees, V = 1483.1(7) Angstrom(3) and Z = 4. The op
en framework delimits one-dimensional 10-ring channels; it is built up
from the hexameric unit Ga-3(PO4)(3)F-2 in which the gallium atoms ex
hibit two types of surrounding. One of the three gallium atoms is octa
hedrally coordinated and the two others are in trigonal bipyramidal co
ordinations where fluorine atoms link the gallium atoms together. Stro
ng hydrogen bonding interactions between the fluorine and the amine fu
nctions of the diamines are evidenced. The structure was examined by P
-31, F-19, N-15 and C-13 solid-state nuclear magnetic resonance spectr
oscopy. Structural relationships with GaAsO4-2 are discussed.