Ionothermal Synthesis and Structure of a New Layered Zirconium Phosphate

A new layered zirconium phosphate material has been synthesized ionothermally using N-ethylpyridinium (Epy) bromide as both the solvent and the template, and its structure has been solved from synchrotron X-ray powder diffraction data using the charge-flipping routine implemented in Superflip. Rietveld refinement coupled with difference electron density map analysis was used to locate the organic cations between the layers. In the final stages of refinement, it became clear that not only ethylpyridinium but also pyridinium ions were present between the zirconium phosphate layers. These findings were then corroborated using elemental analysis, TGA, and solid-state 13C CP/MAS NMR data.