Knowing When To Stop—Trapping Metastable Polymorphs in Mechanochemical Reactions
Publication type: Journal Article
Publication date: 2017-02-06
scimago Q2
wos Q1
SJR: 0.633
CiteScore: 5.6
Impact factor: 3.4
ISSN: 15287483, 15287505
General Chemistry
Condensed Matter Physics
General Materials Science
Abstract
The cocrystal formation of pyrazinamide (PZA) with malonic acid (MA) was studied in situ. The mechanochemical reaction proceeds via conversion of a crystalline intermediate (PZA:MA II) into the thermodynamically more stable form (PZA:MA I) upon further grinding. The information derived from in situ powder X-ray diffraction (PXRD) enabled the isolation of this new metastable polymorph. On the basis of the PXRD data, the crystal structure of the 1:1 cocrystal PZA:MA II was solved. The polymorphs were further characterized and compared by Raman spectroscopy, solid-state NMR spectroscopy, differential thermal analysis/thermogravimetric analysis, and scanning electron microscopy. Our study demonstrates how monitoring mechanochemical reactions by in situ PXRD can direct the discovery and isolation of even short-lived intermediates not yet accessed by conventional methods.
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Metrics
40
Total citations:
40
Citations from 2024:
7
(17%)
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MLA
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GOST
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Kulla H. et al. Knowing When To Stop—Trapping Metastable Polymorphs in Mechanochemical Reactions // Crystal Growth and Design. 2017. Vol. 17. No. 3. pp. 1190-1196.
GOST all authors (up to 50)
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Kulla H., Greiser S., Benemann S., Rademann K., Emmerling F. Knowing When To Stop—Trapping Metastable Polymorphs in Mechanochemical Reactions // Crystal Growth and Design. 2017. Vol. 17. No. 3. pp. 1190-1196.
Cite this
RIS
Copy
TY - JOUR
DO - 10.1021/acs.cgd.6b01572
UR - https://doi.org/10.1021/acs.cgd.6b01572
TI - Knowing When To Stop—Trapping Metastable Polymorphs in Mechanochemical Reactions
T2 - Crystal Growth and Design
AU - Kulla, Hannes
AU - Greiser, Sebastian
AU - Benemann, Sigrid
AU - Rademann, Klaus
AU - Emmerling, Franziska
PY - 2017
DA - 2017/02/06
PB - American Chemical Society (ACS)
SP - 1190-1196
IS - 3
VL - 17
SN - 1528-7483
SN - 1528-7505
ER -
Cite this
BibTex (up to 50 authors)
Copy
@article{2017_Kulla,
author = {Hannes Kulla and Sebastian Greiser and Sigrid Benemann and Klaus Rademann and Franziska Emmerling},
title = {Knowing When To Stop—Trapping Metastable Polymorphs in Mechanochemical Reactions},
journal = {Crystal Growth and Design},
year = {2017},
volume = {17},
publisher = {American Chemical Society (ACS)},
month = {feb},
url = {https://doi.org/10.1021/acs.cgd.6b01572},
number = {3},
pages = {1190--1196},
doi = {10.1021/acs.cgd.6b01572}
}
Cite this
MLA
Copy
Kulla, Hannes, et al. “Knowing When To Stop—Trapping Metastable Polymorphs in Mechanochemical Reactions.” Crystal Growth and Design, vol. 17, no. 3, Feb. 2017, pp. 1190-1196. https://doi.org/10.1021/acs.cgd.6b01572.
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