scholarly journals Structure Determination of Molecular Solids from Powder X-ray Diffraction Data

2014 ◽  
Vol 70 (a1) ◽  
pp. C1557-C1557
Author(s):  
Kenneth Harris
Keyword(s):  
Solid State ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Structural Information ◽  
Powder Xrd ◽  
Computational Techniques ◽  
Molecular Solids ◽  
X Ray Diffraction ◽  
X Ray

Structure determination of organic molecular solids from powder X-ray diffraction (XRD) data [1] is nowadays carried out extensively by researchers in both academia and industry, and the development of new methodology in this field has made particularly significant impact in the pharmaceuticals industry within the last 20 years or so. However, although software for carrying out each stage of the procedure for structure determination from powder XRD data is now readily accessible and relatively straightforward to use, it is essential that the results from such structure determination calculations are subjected to careful scrutiny to confirm that the final structure obtained is actually correct. In this regard, it can be particularly advantageous to augment the analysis of the powder XRD data and to assist the scrutiny of the structural results by considering complementary structural information derived from other experimental and computational techniques. Techniques that can be particularly valuable in this regard include solid-state NMR spectroscopy, energy calculations (either on individual molecules or periodic crystal structures), vibrational spectroscopies, and techniques of thermal analysis (e.g. DSC and TGA). The lecture will give an overview of the current "state of the art" in the structure determination of organic materials from powder XRD data, giving emphasis [2,3] to the opportunities to enhance the structure determination process by making use of information derived from other experimental (especially solid-state NMR) and computational techniques. Recent results will be presented, with emphasis on raising issues of relevance to research on pharmaceutical materials.

scholarly journals Exploiting the Synergy of Powder X-ray Diffraction and Solid-State NMR Spectroscopy in Structure Determination of Organic Molecular Solids

2013 ◽  
Vol 117 (23) ◽  
pp. 12258-12265 ◽  
Author(s):  
Dmytro V. Dudenko ◽  
P. Andrew Williams ◽  
Colan E. Hughes ◽  
Oleg N. Antzutkin ◽  
Sitaram P. Velaga ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Molecular Solids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy

scholarly journals Combination of solid-state NMR, molecular mechanics and DFT calculations for the molecular structure determination of methyl glycoside benzoates

2020 ◽  
Vol 32 (1) ◽  
pp. 297-307
Author(s):  
Łukasz Szeleszczuk ◽  
Tomasz Gubica ◽  
Sebastian Szmeja ◽  
Arkadiusz Ciesielski ◽  
Michał K. Cyrański ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Solid State ◽  
Dft Calculations ◽  
Molecular Mechanics ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Conformational Search ◽  
Methyl Glycoside ◽  
X Ray Diffraction

AbstractA reliable method for molecular structure determination, excluding single-crystal X-ray diffraction (SCXRD), has been applied to six methyl glycoside tetrabenzoates. The proposed method is based on a global conformational search using molecular mechanics and subsequent DFT calculations guided by a solid-state NMR experiment. The accuracy of the applied method has been verified on three methyl glycoside benzoates for which the SCXRD analysis has been completed. It appeared that the calculated conformations of unprivileged energy could be found in the solid state. Bulky substituents (benzoates) exerted less energetically favored interactions in crystals in contrast to isolated molecules. Therefore, solid-state NMR was revealed to be an indispensable approach for choosing credible conformations from the calculated conformations.

Structure determination of β-Pb2ZnF6 by coupling multinuclear solid state NMR, powder XRD and ab initio calculations

2008 ◽  
pp. 6150 ◽  
Author(s):  
Charlotte Martineau ◽  
Franck Fayon ◽  
Christophe Legein ◽  
Jean-Yves Buzaré ◽  
Monique Body ◽  
...  
Keyword(s):  
Solid State ◽  
Ab Initio Calculations ◽  
Ab Initio ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Powder Xrd

Structure determination of the theophylline–nicotinamide cocrystal: a combined powder XRD, 1D solid-state NMR, and theoretical calculation study

CrystEngComm ◽  
2014 ◽  
Vol 16 (15) ◽  
pp. 3141-3147 ◽  
Author(s):  
Ping Li ◽  
Yueying Chu ◽  
Lin Wang ◽  
Robert M. Wenslow ◽  
Kaichao Yu ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Theoretical Calculation ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Powder Xrd ◽  
First Time

The crystal structure of the theophylline–nicotinamide cocrystal is determined for the first time by using a combined multi-technique approach.

Structure Determination for the Crystalline Phase of Triphenyl Phosphite by Means of Multi-Dimensional Solid-State NMR and X-Ray Diffraction

2001 ◽  
Vol 56 (11) ◽  
pp. 1089-1099 ◽  
Author(s):  
Jürgen Senker ◽  
Jens Lüdecke
Keyword(s):  
Solid State ◽  
Structure Determination ◽  
Crystalline Phase ◽  
Solid State Nmr ◽  
Spin Diffusion ◽  
Rotational Symmetry ◽  
Triphenyl Phosphite ◽  
X Ray Diffraction ◽  
X Ray ◽  
Orientation Of Molecules

The crystalline phase of triphenyl phosphite P(OC6H5)3 was investigated by means of 31P solid-state NMR and X-ray diffraction in a temperature range between 170 K and its melting point (Tm = 293 K). ID MAS NMR spectra exhibit one sharp central resonance indicating only one crystallographically unique molecule in the unit cell. A theoretical analysis concerning the shape of 2D exchange spectra for 1 = 1 /2 nuclei is presented. It is shown that if the exchange is caused by radio-frequency driven spin-diffusion, this technique allows to discriminate rotational symmetry elements in crystalline solids. Used on crystalline triphenyl phosphite, 3-fold symmetry could be revealed clearly. Structure determination based on X-ray single crystal diffraction data collected at 191 K shows that triphenyl phosphite crystallises in hexagonal metric with space group R3̅(wR2= 8.3%, Z = 18) and one molecule in the asymmetric unit. This result is in excellent agreement with the NMR spectroscopic data. The lattice parameters at 200 K were determined to a = 37.887(1) and c = 5.7567(2) Å (V = 7156(1) Å3) by refining an X- ray powder-diffraction pattern. The structure of triphenylphosphite can be described as a close rod packing. The rods are formed by ecliptically arranged triphenylphosphite molecules. Due to the 3-fold rotoinversion axis the orientation of molecules in neighboured rods is antiparallel.

scholarly journals Combining solid state NMR, powder X-ray diffraction, and DFT calculations for CsSc3F10 structure determination

2019 ◽  
Vol 787 ◽  
pp. 1349-1355 ◽  
Author(s):  
Aydar Rakhmatullin ◽  
Mathieu Allix ◽  
Ilya B. Polovov ◽  
Dmitry Maltsev ◽  
Andrey V. Chukin ◽  
...  
Keyword(s):  
Solid State ◽  
Dft Calculations ◽  
Structure Determination ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray
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