Synthesis, characterization and structure determination of a new fluorogallophosphate (Mu-5) prepared in the presence of 1,4,8,11-tetraazacyclotetradecane

A New Organic‐Inorganic Hybrid Gallophosphate Prepared in the Presence of Glycine

“…The gallium source was the oxide β‐Ga 2 O 3 (ICDD 41‐1103) obtained by heating a gallium nitrate solution to 250 °C for 24 h followed by calcination at 1000 °C for 6 h. Tripropylamine (TriPA) (Fluka, purum >98%) was used as a pH modifier. Previous experiments indicated that this amine does not play a templating role in the synthesis of gallophosphates in fluoride media 31. Mu‐32 was obtained by hydrothermal synthesis at 170 °C in a fluoride medium.…”

“…Aluminophosphates and gallophosphates showing such organic‐inorganic bonds are rarely encountered. However, the use of the cyclam molecule (1,4,8,11‐tetraazacyclotetradecane) as a structure‐directing agent in these systems induces the crystallisation of such compounds (STA‐6,29 Cyclam‐Co‐AlPO 4, 30 Mu‐531 and Mu‐632). It was shown, in the AlPO 4 ‐SOD material synthesised in the presence of dimethylformamide, that the organic template is bonded to the inorganic framework via Al−O−C bonds 33.…”

Crystalline oxyfluorinated open-framework compounds: Silicates, metal phosphates, metal fluorides and metal-organic frameworks (MOF)

“…The LTA-type GaPO 4 [55] (Fig. 3) or the gallium phosphates Mu-1 [56], Mu-2 [57], Mu-3 [58], Mu-5 [59] and Mu-15 [60] were obtained by the group of Mulhouse (Patarin) and all these frameworks include the D4R units hosting a fluoride atom. Such a cubic building block was also described in other GaPO 4 solids reported by Morris [61] and Hong [62].…”

NMR analysis of GaPO4 crystal growth in mixtures of phosphoric and sulfuric acids

“…In solid state, the situation is inverted and the predominant species would be that whose presented high degree of condensation. The isotropic 31 P NMR chemical shifts of P(OGa) 4 , P(OGa) 3 , P(OGa) 2 , and P(OGa) groups encountered in some known structures of GaPO 4 based materials appear in the following chemical shift ranges: from À9 to À19 ppm [32][33][34][35][36][37][38][39][40][41][42], À2 to À11 ppm [32,34,38,39,43], À1 to À9 ppm [35,38,43], and +1-0 ppm, [38,43] respectively. This correlation for which 31 P chemical shift in MAS spectra moves in the direction of high field, when an increasing number of gallium surrounds the phosphate, is in agreement with our attribution of liquid state gallophosphate NMR spectra.…”