Evidence of 13 hybrid fluoroaluminates in the composition space diagram of the Al(OH)3–tren–HF–ethanol system |
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| Authors: | Karim Adil Marc Leblanc Vincent Maisonneuve |
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| Institution: | Laboratoire des Oxydes et Fluorures, UMR CNRS 6010, Faculté des Sciences et Techniques, Université du Maine, Avenue Olivier Messiaen, 72085 Le Mans Cedex 09, France |
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| Abstract: | Thirteen phases are now evidenced in the composition space diagram of the Al(OH)3–tren–HF–ethanol system at 190 °C. Solvothermal syntheses are performed under microwave heating. Six new organic–inorganic fluorides crystallise and their structures are determined: (H3O)·H4tren]2·(AlF6)3·6H2O (P-1, Z = 2), H3tren]2·(AlF5(H2O))3·8H2O (C2/c, Z = 8), H3tren]4·(AlF6)2·(Al2F11)·(F)·10H2O (P21/n, Z = 2), H3tren]2·(Al4F18)·3.5H2O (P63, Z = 2), H3tren]2·(Al4F18) (P-1, Z = 1), and H3tren]4·(Al8F35)·(OH)·H2O (P-1, Z = 1). The existence domains are approximately located for all phases. Tren amine is tetraprotonated at high HF concentration, otherwise it is triprotonated. A protonated water cluster, H3O+(H2O)6, appears in (H3O)·H4tren]2·(AlF6)3·6H2O while a new Al4F18 unit, found in H3tren]2·(Al4F18), is evidenced; it results from corner and edge sharing association of four AlF6 octahedra. Finally, the structure of H3tren]4·(Al8F35)·(OH)·H2O revealed the largest known fluoroaluminate polyanion, built from eight vertex sharing AlF6 octahedra, (Al8F35)11−. |
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| Keywords: | Fluoroaluminates Hybrid fluorides Hydrothermal synthesis Microwave heating |
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