Powder crystallography of pharmaceutical materials by combined crystal structure prediction and solid-state 1H NMR spectroscopy

Baias, Maria; Widdifield, Cory M.; Dumez, Jean‐Nicolas; Thompson, Hugh P. G.; Cooper, Timothy G.; Salager, Elodie; Bassil, Sirena; Stein, Robin S.; Lesage, Anne; Day, Graeme M.; Emsley, Lyndon

doi:10.1039/c3cp41095a

Cited by 158 publications

(253 citation statements)

References 70 publications

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“…We have demonstrated that the combined use of 14 160 where structural predictions can be made with computational methods including ab initio random structural searching (AIRSS) algorithm [161][162][163][164] and other algorithms, [165][166][167] and refined with the aid of high-quality NMR data.…”

Section: Discussionmentioning

confidence: 99%

Natural abundance ¹⁴N and ¹⁵N solid-state NMR of pharmaceuticals and their polymorphs

Veinberg

Johnston

Jaroszewicz

et al. 2016

Phys. Chem. Chem. Phys.

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Section: Discussionmentioning

confidence: 99%

Natural abundance ¹⁴N and ¹⁵N solid-state NMR of pharmaceuticals and their polymorphs

Veinberg

Johnston

Jaroszewicz

et al. 2016

Phys. Chem. Chem. Phys.

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“…This approach has come to be known as NMR crystallography. 36,37 Spin diffusion data have been used to determine the crystal packing of organic molecules, 38−40 and 1 H chemical shifts have been used either explicitly 41 or as a crystal structure selection parameter 42,43 when performing computational crystal structure predictions. Information concerning the connectivity in zeolites 44,45 and aluminophosphates 46−48 has also been used to solve the crystal structure of framework systems ab initio.…”

Section: ■ Introductionmentioning

confidence: 99%

Zero Thermal Expansion in ZrMgMo₃O₁₂: NMR Crystallography Reveals Origins of Thermoelastic Properties

et al. 2015

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ABSTRACT:The coefficient of thermal expansion of ZrMgMo 3 O 12 has been measured and was found to be extremely close to zero over a wide temperature range including room temperature (α = (1.6 ± 0.2) × 10 −7 K −1 from 25 to 450°C by X-ray diffraction (XRD)). ZrMgMo 3 O 12 belongs to the family of AMgM 3 O 12 materials, for which coefficients of thermal expansion have previously been reported to range from low-positive to low-negative. However, the low thermal expansion property had not previously been explained because atomic position information was not available for any members of this family of materials. We determined the structure of ZrMgMo 3 O 12 by nuclear magnetic resonance (NMR) crystallography, using 91 Zr, 25 Mg, 95 Mo, and 17 O magic angle spinning (MAS) and 17 O multiple quantum MAS (MQMAS) NMR in conjunction with XRD and density functional theory calculations. The resulting structure was of sufficient detail that the observed zero thermal expansion could be explained using quantitative measures of the properties of the coordination polyhedra. We also found that ZrMgMo 3 O 12 shows significant ionic conductivity, a property that is also related to its structure.

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“…Of the two possible configurations, the syn form with a mirror plane running along the center of the phenazine motif was approximately 10 kcal mol −1 less stable than the anti form that had a twofold axis 7. This was the first step in our approach.…”

mentioning

confidence: 95%

A Hybrid Solid‐State NMR and Electron Microscopy Structure‐Determination Protocol for Engineering Advanced para‐Crystalline Optical Materials

Thomas¹,

Rombouts

Oostergetel

et al. 2017

Chemistry A European J

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Hybrid magic‐angle spinning (MAS) NMR spectroscopy and TEM were demonstrated for de novo structure determination of para‐crystalline materials with a bioinspired fused naphthalene diimide (NDI)–salphen–phenazine prototype light‐harvesting compound. Starting from chiral building blocks with C 2 molecular symmetry, the asymmetric unit was determined by MAS NMR spectroscopy, index low‐resolution TEM diffraction data, and resolve reflection conditions, and for the first time the ability to determine the space group from reciprocal space data using this hybrid approach was shown. Transfer of molecular C 2 symmetry into P2/c packing symmetry provided a connection across length scales to overcome both lack of long‐range order and missing diffraction‐phase information. Refinement with heteronuclear distance constraints confirmed the racemic P2/c packing that was scaffolded by molecular recognition of salphen zinc in a pseudo‐octahedral environment with bromide and with alkyl chains folding along the phenazine. The NDI light‐harvesting stacks ran orthogonal to the intermolecular electric dipole moment present in the solid. Finally, the orientation of flexible lamellae on an electrode surface was determined.

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Powder crystallography of pharmaceutical materials by combined crystal structure prediction and solid-state 1H NMR spectroscopy

Cited by 158 publications

References 70 publications

Natural abundance ¹⁴N and ¹⁵N solid-state NMR of pharmaceuticals and their polymorphs

Natural abundance ¹⁴N and ¹⁵N solid-state NMR of pharmaceuticals and their polymorphs

Zero Thermal Expansion in ZrMgMo₃O₁₂: NMR Crystallography Reveals Origins of Thermoelastic Properties

A Hybrid Solid‐State NMR and Electron Microscopy Structure‐Determination Protocol for Engineering Advanced para‐Crystalline Optical Materials

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Powder crystallography of pharmaceutical materials by combined crystal structure prediction and solid-state 1H NMR spectroscopy

Cited by 158 publications

References 70 publications

Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs

Natural abundance 14N and 15N solid-state NMR of pharmaceuticals and their polymorphs

Zero Thermal Expansion in ZrMgMo3O12: NMR Crystallography Reveals Origins of Thermoelastic Properties

A Hybrid Solid‐State NMR and Electron Microscopy Structure‐Determination Protocol for Engineering Advanced para‐Crystalline Optical Materials

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Product

Resources

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Natural abundance ¹⁴N and ¹⁵N solid-state NMR of pharmaceuticals and their polymorphs

Natural abundance ¹⁴N and ¹⁵N solid-state NMR of pharmaceuticals and their polymorphs

Zero Thermal Expansion in ZrMgMo₃O₁₂: NMR Crystallography Reveals Origins of Thermoelastic Properties