X pert3 powder xrpd

Example 10

Compound I Form F was obtained via slurry of Compound I calcium salt hydrate Form A in MEK at room temperature.

A. X-Ray Powder Diffraction

XRPD was performed with a Panalytical X'Pert³ Powder XRPD on a Si zero-background holder. The 20 position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I Form F is shown in FIG. 16 and summarized in Table 21.

Compound I Form F is characterized by the following elemental analysis Table:

Example 14

Compound I calcium salt EtOH solvate Form C was obtained via slurry of Compound I calcium salt amorphous form in EtOH/H₂O (9:1, v:v) at room temperature.

A. X-Ray Powder Diffraction

XRPD on Compound I calcium salt EtOH solvate Form C was performed with a Panalytical X'Pert³ Powder XRPD on a Si zero-background holder. The 2 theta position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I calcium salt EtOH solvate Form C is shown in FIG. 20 and summarized in Table 25.

Example 24

Compound I calcium salt cyclopentyl methyl ether (CPME) solvate Form A was obtained via slurry of Compound I calcium salt Form A in IPA/CPME (1:1, v/v) at room temperature.

A. X-Ray Powder Diffraction

XRPD was performed with a Panalytical X'Pert³ Powder XRPD on a Si zero-background holder. The 20 position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I calcium salt CPME solvate Form A is shown in FIG. 33 and summarized in Table 41.

Example 23

Compound I calcium salt 1,2-dimethoxyethane solvate Form B was obtained via slurry of Compound I calcium salt hydrate Form A in 1,2-dimethoxyethane at room temperature.

A. X-Ray Powder Diffraction

XRPD was performed with a Panalytical X'Pert³ Powder XRPD on a Si zero-background holder. The 20 position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I calcium salt 1,2-dimethoxy ethane solvate Form B is shown in FIG. 32 and summarized in Table 40.

Example 11

Compound I calcium salt hydrate Form G was obtained via fast cooling of Compound I calcium salt hydrate Form A solution in EtOH:H₂O (v:v, 90:10).

A. X-Ray Powder Diffraction:

XRPD was performed with a Panalytical X'Pert³ Powder XRPD on a Si zero-background holder. The 2 theta position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I calcium salt hydrate Form G is shown in FIG. 17 and summarized in Table 22.

Example 9

Compound I calcium Form E was obtained via solid vapor diffusion of Compound I calcium salt hydrate Form A in EtOAc.

A. X-Ray Powder Diffraction:

XRPD was performed with a Panalytical X'Pert3 Powder XRPD on a Si zero-background holder. The 2 theta position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I calcium salt hydrate Form E is shown in FIG. 15 and summarized in Table 20.

Example 13

Compound I calcium salt EtOH solvate Form B was obtained via temperature cycling between 60° C. and 5° C. with cooling rate of 0.2° C./min of Compound I calcium salt hydrate Form A in EtOH: n-heptane (1:1, v:v).

A. X-Ray Powder Diffraction

Compound I calcium salt EtOH solvate Form B XRPD was performed with a Panalytical X'Pert³ Powder XRPD on a Si zero-background holder. The 2 theta position was calibrated against a Panalytical Si reference standard disc. The XRPD diffractogram for Compound I calcium salt EtOH solvate Form A is shown in FIG. 19 and summarized in Table 24.