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.