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The reaction of molybdophosphoric acid with zinc carbonate followed by addition of hmta leads to formation of a triclinic polymorph of bis (3,5,7-triaza-1-azoniatricyclo[3.3.1.1 3,7 ]decane) bis(μ 4 -oxo)-tris(μ 3 -oxo)-nonakis(μ 2 -oxo)-nonaaqua-decaoxohepta-molybdenum-di-zinc(II) dihydrate in a one pot simple reaction. The obtained compound has been characterised by IR, UV-Vis spectroscopy, elemental analysis, and X-ray crystallography. A detailed comparison between both polymorphic forms: triclinic a = 22.758Å, b = 24.702Å, c = 31.995Å, α = 101.206• , β = 103.256• , and V = 16203.8Å 3 and monoclinic a = 43.120Å, b = 12.399Å, c = 16.285Å, α = 90.00• , β = 111.12 • , γ = 90.00• , and V = 8122Å 3 was performed. The influence of the synthesis procedure on polymorph formation was described.

KEYWORDSTwo amino acids, leucine and valine, were studied by X-ray powder diffraction (XRPD). The linear correlations between intensity of racemate (decrease) or enantiomer (increase) and enantiomeric excesses were observed in each case.Leucine Valine Enantiomeric excess X-ray powder diffraction