Untersuchungen der Hydroxylammonium-Fluorozirconate(IV)

Summary

Hydroxylammonium fluorozirconates have been investigated. Two new microcristalline phases have been isolated from aqueous solutions: (NH₃OH)₂ZrF₆ (1) and (NH₃OH)₃ZrF₇ (2). The crystals were prepared by slow evaporation of the solution of NH₂OH, Zr, and HF. Different compositions of the crystals were achieved by varying the molar ratios of the components. They were characterized by thermal analysis, vibrational spectroscopy, and structure (single crystal x-ray methods). (NH₃OH)₂ZrF₆ (1) crystallizes triclinic, P$\overline 1$ (No.: 2),a=7.400(2),b=7.609(2),c=7.887(2) Å, α=57.29(3)°, β=62.16(3)°, γ=67.83(2)°. (NH₃OH)₃ZrF₇ (2) crystallizes triclinic, P$\overline 1$ (No.: 2),a=7.128(1),b=7.989(1),c=8.888(1) Å, α=109.72(1)°, β=91.01(1)°, γ=104.27(1)°.