Abstract: | The title compound, (H3O)2NaAl3F12 dihydronium sodium trialuminum(III) dodecafluoride], was obtained by solvothermal synthesis from the reaction of aluminium hydroxide, sodium hydroxide, 1,2,4‐triazole and aqueous HF in ethanol at 463 K for 48 h. The structure consists of AlF6 octahedra organized in AlF4−]n HTB‐type sheets (HTB is hexagonal tungsten bronze) separated by H3O+ and Na+ cations. |