Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 1. (A) Molecular structure of POSA; and (B) An illustration of representative molecular packings in POSA Form I.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 2. DSC thermograms (A) and PXRD patterns (B) of POSA Form I, III, and c.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 3. 1D 13C CP spectra of three POSA polymorphs. All spectra were acquired under 12 kHz MAS and 9.4 Tesla magnetic field.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 4. Probing structures of POSA polymorphs from 1D 1H spectra. (A) Sensitivity and resolution enhancement of 1H spectra of POSA Form I at higher MAS frequencies; (B) 1D 1H spectra of polymorphic forms of POSA under a MAS frequency of 100 kHz; and (C) A representative molecular structure showing intermolecular hydrogen bonding between H44 and carbonyl group in Form I. All spectra were acquired at 16.5 Tesla magnetic field and various MAS frequencies in (A) and 100 kHz in (B).

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 5. 2D 1H–13C HETCOR spectra of POSA Form I with the CP contact time of 100 ls (A) and 1000 ls (B). 1D 1H and 13C slices of C16-H16 cross peak are shown in (A) to illustrate 1H and 13C linewidths. 1H projections of the direct dimension are shown on the top of the 2D spectra. All spectra were acquired under 100 kHz MAS and 16.5 Tesla magnetic field.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 6. 2D 1H DQ-SQ correlation spectra of POSA Form I (A), Form III (B), and Form c (C). (D) 1D cross sections of H51, H46/47, and H44 extracted from each 2D spectra of the three polymorph forms. All spectra were acquired under 100 kHz MAS and 16.5 Tesla magnetic field.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 7. 2D 1H–1H RFDR spectra (A–E) of POSA Form I acquired with different mixing times ranging from 0.5 to 8 ms; and extracted 1H 1D slices of H44 (F) and H51 (G). All spectra were acquired under 100 kHz MAS and 16.5 Tesla magnetic field.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 8. Molecular packing from 1H–1H RFDR build-up curves of three POSA polymorphs: intramolecular contacts of H38–H44 (A) and H49/51–H46/47 (B); and intermolecular contacts of H49/51–H16 (C) and H44–H49/51 (D).

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques:

Journal: Journal of magnetic resonance (San Diego, Calif. : 1997)

Article Title: Ultrafast magic angle spinning NMR characterization of pharmaceutical solid polymorphism: A posaconazole example.

doi: 10.1016/j.jmr.2022.107352

Figure Lengend Snippet: Fig. 9. (A) Intermolecular packing of POSA Form I and (B) A hypothetical packing model of POSA Form c.

Article Snippet: The naturally abundant POSA Form I, III, and cwere synthesized by Merck & Co., Inc. Rahway, NJ 07065, USA following previously published procedures [59].

Techniques: