Annie Hémon-Ribaud

ZnAlF5·[TAZ]: an Al fluorinated MOF of MIL-53(Al) topology with cationic {Zn(1,2,4 triazole)}2+ linkers

ZnAlF5·[TAZ], the first aluminium fluorinated metal–organic framework with cationic {Zn(1,2,4 triazole)}2+ linkers has been synthesized. The structure is accurately determined by coupling direct space methods on laboratory powder X-ray diffraction data with solid-state nuclear magnetic resonance experiments and ab initio calculations, and is found to be analogous to that of MIL-53(Al).

Synthesis, Crystal Structure, and Characterization of a New Adduct 3-Ammoniumphenyl Sulfone Dihydrogenphosphate Phosphoric Acid [C12H14N2SO2](H2PO4)2H3PO4

Abstract A new adduct 3-ammoniumphenyl sulfone dihydrogenphosphate phosphoric acid, [C12H14N2O2S](H2PO4)2H3PO4, has been synthesized by slow evaporation at room temperature using 3-aminophenyl sulfone as the structure-directing agent. The structure, determined by single-crystal X-ray diffraction at 293 K, can be described as inorganic layers built by H2PO4 − groups and H3PO4 molecules, parallel to the (a, c) planes at y = 0.5, between which molecules of the organic group [C12H14N2O2S]2+ are inserted. In this atomic arrangement, hydrogen bonds and van der Waals interactions between the different species play an important role in the tri-dimensional network cohesion. Solid-state 13C and 31P MAS NMR spectroscopies are in agreement with the X-ray structure. [Supplemental materials are available for this article. Go to the publishers online edition of Phosphorus, Sulfur, and Silicon and the Related Elements for the following free supplemental resource: Tables S1 and S2. Figures S1 and S2.] GRAPHICAL ABSTRACT

On new fluorides with the Jarlite-type structure: crystal structures of Na2Sr7Al6F34, Na2Sr6ZnFe6F34 and Ba7Ga6(F,OH)32 · 2H2O

Abstract New compounds, Na 2 Sr 7 Al 6 F 34 , Na 2 Sr 6 ZnFe 6 F 34 and Ba 7 Ga 6 (F,OH) 32 · 2H 2 O, have been prepared by hydrothermal synthesis in HF solution and by the chloride flux method. The crystal structures have been resolved by X-ray diffraction. All the phases present structures of the Jarlite type in spite of having a different unit cell for the iron phase. The structures of the two first compounds are characterized by [Na 2 Al 6 F 34 ] n 14 n − or [NaZnFe 6 F 34 n 13 n − sheets of octahedra connected by Sr or [Sr, Na] polyhedra whereas the hydrated fluoride exhibits [Ga 3 (F,OH) 16 ] 7− isolated octahedra trimers separated by Ba ions and water molecules. Structural correlations are made with other Jarlite type phases and with structures involving ‘independent’ fluoride ions.

2,4,6-Triamino-1,3,5-triazine-1,3-diium aqua-penta-fluoridoaluminate.

The title compound, (C3H8N6)[AlF5(H2O)], was obtained by solvothermal synthesis from the reaction of aluminium hydroxide, 1,3,5-triazine-2,4,6-triamine (melamine), aqueous HF and water at 323 K for 48 h. The structure consists of [AlF5(H2O)]2− octahedra and diprotonated melaminium cations. Cohesion is ensured by a three-dimensional network of hydrogen bonds.

(H3O)2NaAl3F12, isostructural with A2NaAl3F12 (A = K+, Rb+, Cs+) fluorides having HTB‐type sheets

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.

Bis(butane-1,4-diammonium) di-μ-oxido-bis[trifluoridooxidomolybdate(V)] monohydrate.

The title compound, (C4H14N2)2[Mo2O4F6]·H2O, was obtained by solvothermal reaction at 443 K for 72 h from a mixture of MoO3, HF, 1,4-diaminobutane (dab), water and ethylene glycol. The structure consists of [Mo2O4F6]4− anionic dimers containing strongly distorted MoO3F3 octahedra (with twofold symmetry), diprotonated dab cations and water molecules (twofold symmetry) in the ratio 1:2:1. The cohesion of the three-dimensional structure is ensured through N—H⋯O, N—H⋯F and O—H⋯F interactions.