Na3SO4H-The First Representative of the Material Class of Sulfate Hydrides

The first representative of a novel class of mixed-anionic compounds, the sulfate hydride Na3SO4H, and the corresponding deuteride Na3SO4D were obtained from the solid-state reaction of NaH or NaD with dry Na2SO4. Precise reaction control is required, because too harsh conditions lead to the reduction of sulfate to sulfide. A combined X-ray and neutron diffraction study revealed that the compound crystallizes in the tetragonal space group P4/nmm with the lattice parameters a=7.0034(2) angstrom and c=4.8569(2) angstrom. The sole presence of hydride and absence of hydroxide ions is proven by vibrational spectroscopy and comparison with spectra predicted from quantum chemical calculations. H-1 and Na-23 MAS NMR spectra are consistent with the structure of Na3SO4H: a single H-1 peak at 2.9 ppm is observed, while two peaks at 15.0 and 6.2 ppm for the inequivalent Na-23 sites are observed. Elemental analysis and quantum chemical calculations further support these results.

Automated summary

A novel mixed-anionic compound, the sulfate hydride Na3SO4H, was successfully synthesized by precise reaction control to prevent the reduction of sulfate to sulfide. X-ray and neutron diffraction studies revealed its crystalline structure and properties.