Solvothermal preparation, characterization by IR absorption, DTA-TG analysis, X-ray thermodiffraction and crystal structure determination are reported for a new fluoride zirconate (C8H12N)4•Zr2F12. The cell is monoclinic (P21/a ; Z = 2) with a = 14.407(2) Å ; b = 7.727(3) Å ; c = 17.37(4) Å and β = 94.83(6)°. The structure solution is refined to R = 0.025 and Rw = 0.079 using 2789 independent reflections. The 3D arrangement consists of (001) layers of Zr2F12 dimers and phenylethylammonium cations in which organic cations are linked to fluoride ions by N-H…F hydrogen bonds. The interlayer Van der Waals interactions are weak and the thermal stability of the structure is poor. Thermal analysis and X-ray thermodiffraction reveal a phase transition at T ≈ 100°C before the decomposition starts at T ≈ 120°C and ends at T ≈ 350°C to give ZrF4.
I. Balti, T. Ben Chaabane, M. Leblanc, A. Ben Ali
Solvothermal, XRD, crystal structure, hybrid