X-ray powder diffraction (XRPD) and X-ray radial electronic distribution density (RED) of initial and zirconia-pillared interlayered clays (Zr-PILC) were studied. After pillaring, the basal (001) spacing was found to increase from 11 Angstrom in the initial clay kept under air to 17.7 Angstrom in Zr-PILC. The structure of zirconium nanopillars was characterized. The interatomic distances with corresponding coordination numbers obtained from the RED curves were close to those in zirconium tetramers.