Ga 4 (PO 4 ) 4 F·N 2 C 7 H 11 · 1 / 2 H 2 O was prepared solvothermally in pure form using 4-(dimethylamino)pyridine (4-DMAP) as a template in various solvents (pyridine, pyridine/water, and ethylene glycol) within a broad reaction temperature range (115−180 °C). Its structure was determined from X-ray single-crystal diffraction data at low temperature (−105 °C). Ga 4 (PO 4 ) 4 F·N 2 C 7 H 11 · 1 / 2 H 2 O crystallizes in the monoclinic space group C 2/ c, with a = 22.093(4) Å, b = 13.904(2) Å, c = 14.230(2) Å, β = 98.431(3)°, V = 4324 Å 3, and Z = 8. Its three-dimensional framework is composed of novel distorted “bowl-shaped” octameric double 4-ring units, which are built up by corner-sharing PO 4 and GaO 4 tetrahedra and GaO 4 F trigonal bipyramids. The structure consists of a pseudohexagonal array of cylindrical 12-membered pores running parallel to the c axis hosting the protonated 4-DMAP molecules. These pores are interconnected along the b axis through double 8-ring windows. The framework remains stable up to 300 °C under oxygen.
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Bonhomme et al. (2001) studied this question.