Polymorph Selection via Sublimation onto Siloxane Templates

Solomos, Marina A.; Capacci-Daniel, Christina; Rubinson, Judith F.; Swift, Jennifer A.

doi:10.1021/acs.cgd.8b01151

Cited by 13 publications

(16 citation statements)

References 57 publications

(64 reference statements)

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“…Previous work has demonstrated that it is possible to template the growth of a particular form and discover new polymorphs by subliming onto different surfaces, e.g ., polycrystalline powders, 76 siloxane-coated glass, 65 and crystals with related structure. 32 , 33 Both Forms I and II of IPN display different hydrogen bonding patterns to the known form of ISN and hence crystals of one compound could be used to template the growth of new forms of the other analogue.…”

Section: Resultsmentioning

confidence: 99%

Minimizing Polymorphic Risk through Cooperative Computational and Experimental Exploration

et al. 2020

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We combine state-of-the-art computational crystal structure prediction (CSP) techniques with a wide range of experimental crystallization methods to understand and explore crystal structure in pharmaceuticals and minimize the risk of unanticipated late-appearing polymorphs. Initially, we demonstrate the power of CSP to rationalize the difficulty in obtaining polymorphs of the well-known pharmaceutical isoniazid and show that CSP provides the structure of the recently obtained, but unsolved, Form III of this drug despite there being only a single resolved form for almost 70 years. More dramatically, our blind CSP study predicts a significant risk of polymorphism for the related iproniazid. Employing a wide variety of experimental techniques, including high-pressure experiments, we experimentally obtained the first three known nonsolvated crystal forms of iproniazid, all of which were successfully predicted in the CSP procedure. We demonstrate the power of CSP methods and free energy calculations to rationalize the observed elusiveness of the third form of iproniazid, the success of high-pressure experiments in obtaining it, and the ability of our synergistic computational-experimental approach to “de-risk” solid form landscapes.

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Section: Resultsmentioning

confidence: 99%

Minimizing Polymorphic Risk through Cooperative Computational and Experimental Exploration

et al. 2020

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“…In turn, Patel et al in their paper described a new method called Predicting Efficacy Through Intermolecular Interactions (PETI) for predicting the effectiveness of different polymer surfaces in promoting heterogeneous nucleation [ 24 ]. Solomos et al crystallized diphenylurea via slow evaporation from a range of solvents [ 25 ]. The experiments demonstrated the utility of template-directed sublimation methods as a way to obtain metastable phases with high phase purity.…”

Section: Basic Researchmentioning

confidence: 99%

Application of Polymers as a Tool in Crystallization—A Review

et al. 2021

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The application of polymers as a tool in the crystallization process is gaining more and more interest among the scientific community. According to Web of Science statistics the number of papers dealing with “Polymer induced crystallization” increased from 2 in 1990 to 436 in 2020, and for “Polymer controlled crystallization”—from 4 in 1990 to 344 in 2020. This is clear evidence that both topics are vivid, attractive and intensively investigated nowadays. Efficient control of crystallization and crystal properties still represents a bottleneck in the manufacturing of crystalline materials ranging from pigments, antiscalants, nanoporous materials and pharmaceuticals to semiconductor particles. However, a rapid development in precise and reliable measuring methods and techniques would enable one to better describe phenomena involved, to formulate theoretical models, and probably most importantly, to develop practical indications for how to appropriately lead many important processes in the industry. It is clearly visible at the first glance through a number of representative papers in the area, that many of them are preoccupied with the testing and production of pharmaceuticals, while the rest are addressed to new crystalline materials, renewable energy, water and wastewater technology and other branches of industry where the crystallization process takes place. In this work, authors gathered and briefly discuss over 100 papers, published in leading scientific periodicals, devoted to the influence of polymers on crystallizing solutions.

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“…60 As a result, sublimation experiments were also undertaken as they have previously been used to crystallize the formation of metastable forms. [61][62][63] ISN was sublimed by heating on a microscope stage below its melting point (171.4°C) at relatively high heating rates (5 and 10 °C/min). A borosilicate glass coverslip was placed above the sample and the ISN vapour crystallized on the colder coverslip.…”

Section: Experimental Crystallization Of Isn and Ipnmentioning

confidence: 99%

“…Previous work has demonstrated that it is possible to template the growth of a particular form and discover new polymorphs by subliming onto different surfaces, e.g. polycrystalline powders, 71 siloxane-coated glass 61 and crystals with related structure. 32,33. Both Forms I and II of IPN display different hydrogen bonding patterns to the known form of ISN and hence crystals of one compound could be used to template the growth of new forms of the other analogue.…”

Section: Templated Sublimationsmentioning

confidence: 99%

Minimizing Polymorphic Risk Through Cooperative Computational and Experimental Exploration

Taylor¹,

Mulvee²,

Perenyi³

et al. 2020

Preprint

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<div> <p>We combine state-of-the-art computational crystal structure prediction (CSP) techniques with a wide range of experimental crystallization methods to understand and explore crystal structure in pharmaceuticals and minimize the risk of unanticipated late-appearing polymorphs. Initially, we demonstrate the power of CSP to rationalize the difficulty in obtaining polymorphs of the well-known pharmaceutical isoniazid and show that CSP provides the structure of the recently discovered, but unsolved, Form III of this drug despite there being only a single known form for almost 70 years. More dramatically, our blind CSP study predicts a significant risk of polymorphism for the related iproniazid. Employing a wide variety of experimental techniques, including high-pressure experiments, we experimentally obtained the first three known non-solvated crystal forms of iproniazid, all of which were successfully predicted in the CSP procedure. We demonstrate the power of CSP methods and free energy calculations to rationalize the observed elusiveness of the third form of iproniazid, the success of high-pressure experiments in obtaining it, and the ability of our synergistic computational-experimental approach to “de-risk” solid form landscapes.</p> </div>

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Polymorph Selection via Sublimation onto Siloxane Templates

Cited by 13 publications

References 57 publications

Minimizing Polymorphic Risk through Cooperative Computational and Experimental Exploration

Minimizing Polymorphic Risk through Cooperative Computational and Experimental Exploration

Application of Polymers as a Tool in Crystallization—A Review

Minimizing Polymorphic Risk Through Cooperative Computational and Experimental Exploration

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