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Dalton Trans. 2016 May 4;45(18):7616-26. doi: 10.1039/c6dt00734a.

Microporous aluminophosphates synthesized with 1,2,3-trimethylimidazolium and fluoride.

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Center for Ordered Nanoporous Materials Synthesis, School of Environmental Science and Engineering, POSTECH, Pohang 790-784, Korea.
Departamento de Química Física, Universidad del País Vasco (UPV/EHU), Apartado 644, 48080, Bilbao, Spain.
Instituto de Ciencia de Materiales de Madrid (ICMM), Consejo Superior de Investigaciones Científicas (CSIC), Sor Juana Inés de la Cruz 3, 28039 Madrid, Spain.


The synthesis of microporous aluminophosphates using 1,2,3-trimethylimidazolium (123TMI) and fluoride produces three phases (HPM-3, PST-27 and triclinic AlPO4-34) depending on the amount of water and organic structure-directing agents in the synthesis mixture. Fluoride occluded in double 4-ring units was not detected by (19)F MAS NMR spectroscopy in any product. While the structure of HPM-3 remains unknown, PST-27 has been determined to be a monoclinic version of AlPO4-5 with a distorted and likely complex structure. Rietveld analysis using synchrotron diffraction data for as-made triclinic AlPO4-34 reveals that each of its cha-cages holds two 123TMI cations, forming a displaced anti-parallel dimer with a short distance between aromatic rings (3.78 Å from center to center, 3.63 Å from plane to plane). This suggests that π-π interactions may play a role in the synthesis of this phase and related CHA-type systems. A study of the optical properties of PST-27, AlPO4-34 and other materials containing 123TMI cations shows their complex fluorescence behavior, sometimes displaying a red-edge effect, i.e., a red shift of the fluorescence as the excitation wavelength is shifted toward the red edge of the absorption band. An absorption band at 291 nm appears only in the dimer-containing triclinic AlPO4-34 and is sensitive to the introduction of Si into the framework.


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