Selective polymorph transformation via solvent-drop grinding

Chemical Communications

Volumn , Issue 7, 2005, Pages 880-882

  Trask, Andrew V ^a   Shan, Ning ^b   Motherwell, W D Samuel ^c   Jones, William ^a   Feng, Shaohua ^b   Tan, Reginald B H ^b   Carpenter, Keith J ^b  

^a UNIVERSITY OF CAMBRIDGE   (United Kingdom)

^b INSTITUTE OF CHEMICAL AND ENGINEERING SCIENCES   (Singapore)

^c CAMBRIDGE CRYSTALLOGRAPHIC DATA CENTRE   (United Kingdom)

Author keywords

[No Author keywords available]

Indexed keywords

ADSORPTION; ARTICLE; CHEMICAL REACTION; CRYSTALLIZATION; ENVIRONMENTAL TEMPERATURE; GRINDING; HIGH TEMPERATURE; PHYSICAL CHEMISTRY; TEMPERATURE DEPENDENCE; X RAY POWDER DIFFRACTION;

EID: 14644399220     PISSN: 13597345     EISSN: None     Source Type: Journal    
DOI: 10.1039/b416980h     Document Type: Article

References (26)

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14. In a strict sense, form I is a mixed crystal of neutral and zwitterionic AA molecules, and a polymorphic relationship to forms II and III could be debated. It will be termed a polymorph here, according to the convention of literature regarding AA crystal forms.
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18. All PXRD described herein were collected at ambient temperature with a Philips X'Pert diffractometer using Cu Kα radiation and an X'Celerator detector.
19. Reference PXRD patterns were simulated from the previously reported crystal structures with the software package X'Pert Plus, Philips Analytical B.V., Version 1.0, using the following structures in the Cambridge Structural Database (CSD): α-SA: SUCACB07; β-SA: SUCACB06; AA-I: AMBACO07; AA-II: AMBACO08; AA-III: AMBACO03.
20. All grinding experiments described herein were performed with a Retsch MM200 Mixer Mill with 10 ml stainless steel grinding jars and one 7 mm stainless steel grinding ball per jar. 100 mg crystalline powder was ground at a rate of 30 Hz. Solvent additions were in the quantity of four drops from a pipette (ca. 0.1 ml).
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23. Private communication to CSD; Refcode SUCACB07, see www.ccdc.cam.ac.uk.
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25. Careful examination of PXRD patterns in conjunction with differential scanning calorimetry measurements revealed that commercially available SA contained trace amounts of the unstable α-SA polymorph. Recrystallized samples contained a smaller trace amount of α-SA, the quantity of which is too minor to be observed in Fig. 3. The limit of detection of PXRD is typically considered to be on the order of 5%.
26. In addition to solvent-induced defect formation, the presence of small amounts of crystalline or amorphous impurities (below the detection limit of PXRD) may also be important.