Slow evaporation in a variety of commonly used solvents (ranging from apolar to polar aprotic and polar protic) was employed for polymorph screening for all eight compounds,36 and high-quality single crystals were used for structure determination by SCXRD. The identity of individual batches of crystals was determined by PXRD.
The crystallographic data of all crystal forms were collected on a Rigaku Oxford diffractometer at ambient temperatures, except for 1-I, for which data collection was carried out on a Bruker APEX-II diffractometer with a CuKα radiation (λ = 1.54184 Å). Cell refinement and data reduction were performed using CrysAlisPro. Structure solution and refinement were carried out using the SHELXT37 and SHELXL38 (link) programs, respectively. PXRD data for the crystal forms were collected on a Rigaku X-ray diffractometer with CuKα radiation (40 kV, 15 mA, λ = 1.5406 Å) between 5.0 and 50.0° (2θ) at ambient temperatures.
DSC experiments were performed on SII instruments DSC6220 (Seiko Instruments Inc., Japan). TGA experiments were run on SDT Q600 (TA Instruments, USA). Tzero® pans and aluminum hermetic lids were used for measuring a few milligrams of a finely ground sample, at a heating rate of 10 °C min−1.
The crystallographic data of all crystal forms were collected on a Rigaku Oxford diffractometer at ambient temperatures, except for 1-I, for which data collection was carried out on a Bruker APEX-II diffractometer with a CuKα radiation (λ = 1.54184 Å). Cell refinement and data reduction were performed using CrysAlisPro. Structure solution and refinement were carried out using the SHELXT37 and SHELXL38 (link) programs, respectively. PXRD data for the crystal forms were collected on a Rigaku X-ray diffractometer with CuKα radiation (40 kV, 15 mA, λ = 1.5406 Å) between 5.0 and 50.0° (2θ) at ambient temperatures.
DSC experiments were performed on SII instruments DSC6220 (Seiko Instruments Inc., Japan). TGA experiments were run on SDT Q600 (TA Instruments, USA). Tzero® pans and aluminum hermetic lids were used for measuring a few milligrams of a finely ground sample, at a heating rate of 10 °C min−1.