Hydroxylammonium Tetrafluoridooxidovanadate(V) - (NH3OH)[VOF4]

Area of Science:

• Inorganic Chemistry
• Crystallography
• Materials Science

Background:

• Vanadium oxyfluoride compounds are of interest due to their diverse structural motifs and potential applications.
• Understanding the synthesis and structural properties of novel vanadium complexes is crucial for advancing inorganic chemistry.
• Previous studies have explored various vanadium-oxygen-fluorine systems, but the specific compound hydroxylammonium tetrafluoridooxidovanadate(V) requires detailed investigation.

Purpose of the Study:

• To synthesize hydroxylammonium tetrafluoridooxidovanadate(V) [(NH3OH)[VOF4]].
• To characterize the synthesized compound in the solid state using advanced analytical techniques.
• To elucidate the crystal structure and bonding environment of the title compound.

Main Methods:

• Synthesis via reaction of hydroxylammonium chloride [(NH3OH)Cl] and vanadium oxytrifluoride [VOF3] in anhydrous hydrogen fluoride [HF].
• Solid-state characterization employing single-crystal X-ray diffraction.
• Vibrational spectroscopy using Raman spectroscopy.

Main Results:

• Successful synthesis of colorless hydroxylammonium tetrafluoridooxidovanadate(V) [(NH3OH)[VOF4]].
• Determination of monoclinic crystal structure (space group P21/n) with specific lattice parameters (a = 7.2349(2) Å, b = 5.0351(2) Å, c = 12.8322(4) Å, β = 94.843(3)°, V = 465.79(3) ų, Z = 4 at 150 K).
• Identification of polymeric chain anions [VOF4]nn- interconnected by hydrogen bonds with hydroxylammonium cations (NH3OH)+.

Conclusions:

• The crystal structure of hydroxylammonium tetrafluoridooxidovanadate(V) consists of infinite [VOF4]nn- chains.
• Hydrogen bonding plays a critical role in linking the anionic chains with the organic cations.
• This study provides fundamental structural data for a novel vanadium oxyfluoride complex.