Example 18
Compound I calcium salt acetone solvate Form A was made by slurrying Compound I calcium salt amorphous form in acetone at 4° C. This material was very labile. It quickly dried to Compound I calcium salt hydrate Form C when air-dried.
A. X-Ray Powder Diffraction
X-ray powder diffraction (XRPD) spectra were recorded at room temperature in transmission mode using a PANalytical Empyrean system equipped with a sealed tube source and a PIXcel 1D Medipix-3 detector (Malvern Pa. Nalytical Inc, Westborough, Mass.). The X-Ray generator operated at a voltage of 45 kV and a current of 40 mA with copper radiation (1.54060 Å). The powder sample was placed on a 96-well sample holder with mylar film and loaded into the instrument. The sample was scanned over the range of about 3° to about 40° 2θ with a step size of 0.0131303° and 49 s per step. The XRPD diffractogram for Compound I calcium salt acetone solvate Form A is shown in
