Tetraalkylammonium salts produced micro crystals that are not suitable for x-ray single
crystal diffractions. Structural data can be extracted from powder diffraction patterns and by
use of mathematical methods. The method used for this research based on Rietveld method to
perform full matrix least-squares refinement of unit parameters from powder diffraction
patterns. Powder Diffraction pattern of a number of chromate complexes were successfully
analyzed by mathematical equations. The use of pattern-fitting techniques for the
characterization of the microstructure is discussed through applications to nanocrystalline
materials. We used direct space that need no powder pattern analysis and is based on global
optimization of a structural model to improve agreement between the observed and
calculated diffraction patterns. The extracted data compared with single crystal X-ray data
and found good agreement between two kinds of data.
