The principles underlying the use of powder diffraction data in solving pharmaceutical crystal structures

Shankland, Kenneth; Spillman, Mark J.; Kabova, Elena A.; Edgeley, David S.; Shankland, Norman

doi:10.1107/s0108270113028643

Cited by 30 publications

(32 citation statements)

References 70 publications

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“…For the structures studied in this work, which are of moderate molecular and crystallographic complexity (Shankland et al, 2013), both transmission capillary and transmission flat plate setups are clearly very good options. Whilst the full width at half maximum values are higher for the transmission flat plate setup than for the transmission capillary, provided the PXRD pattern can be indexed, this is not a significant impediment to global-optimisation based SDPD, as implemented in DASH.…”

Section: Discussionmentioning

confidence: 99%

“…Since the late 1990s, developments in crystal structure determination from powder diffraction data (SDPD) methods have meant that it is often relatively straightforward to solve complex molecular crystal structures from laboratory-based PXRD data alone (Kabova et al, 2017;Shankland et al, 2013;Fernandes et al, 2007;Bushmarinov et al, 2012;Chernyshev et al, 2010;Chernyshev et al, 2009) without the need for the high instrumental resolution that a synchrotron source allows. In principle, therefore, SDPD could be much more routinely accessible to the laboratory chemist.…”

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confidence: 99%

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Pushing the Limits of Molecular Crystal Structure Determination From Powder Diffraction Data in High-Throughput Chemical Environments

Kabova

Blundell

Shankland

2018

Journal of Pharmaceutical Sciences

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Crystal structure determination from powder diffraction data (SDPD) using the DASH software package is evaluated for data recorded using transmission capillary, transmission flat plate, and reflection flat plate geometries on a selection of pharmaceutical compounds. We show that transmission capillary geometry remains the best option when crystal structure determination is the primary consideration and, as expected, reflection flat plate geometry is not recommended for SDPD because of preferred orientation effects. However, the quality of crystal structures obtained from transmission plate instruments can be excellent, and the convenience factor for sample preparation, throughput, and retrieval is higher than that of transmission capillary instruments. Indeed, it is possible to solve crystal structures within an hour of a polycrystalline sample arriving in the laboratory, which has clear implications for making small-molecule crystal structures more routinely available to the practicing laboratory medicinal chemist. With appropriate modifications to crystal structure determination software, it can be imagined that SDPD could become a rapid turn-around walk-up analytical service in high-throughput chemical environments.

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Section: Discussionmentioning

confidence: 99%

mentioning

confidence: 99%

Pushing the Limits of Molecular Crystal Structure Determination From Powder Diffraction Data in High-Throughput Chemical Environments

Kabova

Blundell

Shankland

2018

Journal of Pharmaceutical Sciences

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“…A recent review of the principles underlying the structure solution of molecular compounds illustrates the variety of methods applied and the variety of problems that are encountered. In this review two situations are particularly discussed: the presence of impurities and the high crystallographic complexity, i.e.…”

Section: Structure Solution Proceduresmentioning

confidence: 99%

Structure determination from powder diffraction data: past, present and future challenges

Meden

Evans

2015

Crystal Research and Technology

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Structural information is crucial for understanding and tailoring the materials properties. When the materials are available only in the polycrystalline form, powder diffraction is the method of choice for structure determination. Compared to the single crystal data, the powder pattern contains less information due to the overlap problem and the reduction of the information content is even larger if only the low resolution data are available. Several data analysis approaches are available to address this problem, including reciprocal, direct and dual space methods. They are discussed and illustrated by a number of examples, including cases where other techniques, such as IR and NMR spectroscopy, electron microscopy and crystal-chemical knowledge have to be applied to solve the structure.

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“…The addition of a small amount of a solvent in liquid-assisted grinding increases the rate of co-crystallization by a process called solution-mediated phase transformation [6]. However, mechanochemical methods inherently produce only polycrystalline products, and as such, crystal structure determination from powder diffraction data methods [7][8][9][10] has an important role to play in the structural characterization of these products.…”

Section: Introductionmentioning

confidence: 99%

Co-Crystal Structures of Furosemide:Urea and Carbamazepine:Indomethacin Determined from Powder X-Ray Diffraction Data

Rahal

Majumder²,

Spillman

et al. 2020

Crystals

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Co-crystallization is a promising approach to improving both the solubility and the dissolution rate of active pharmaceutical ingredients. Crystal structure determination from powder diffraction data plays an important role in determining co-crystal structures, especially those generated by mechanochemical means. Here, two new structures of pharmaceutical interest are reported: a 1:1 co‑crystal of furosemide with urea formed by liquid-assisted grinding and a second polymorphic form of a 1:1 co‑crystal of carbamazepine with indomethacin, formed by solvent evaporation. Energy minimization using dispersion-corrected density functional theory was used in finalizing both structures. In the case of carbamazepine:indomethacin, this energy minimization step was essential in obtaining a satisfactory final Rietveld refinement.

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The principles underlying the use of powder diffraction data in solving pharmaceutical crystal structures

Cited by 30 publications

References 70 publications

Pushing the Limits of Molecular Crystal Structure Determination From Powder Diffraction Data in High-Throughput Chemical Environments

Pushing the Limits of Molecular Crystal Structure Determination From Powder Diffraction Data in High-Throughput Chemical Environments

Structure determination from powder diffraction data: past, present and future challenges

Co-Crystal Structures of Furosemide:Urea and Carbamazepine:Indomethacin Determined from Powder X-Ray Diffraction Data

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