Structural investigations of three triazines: solution-state NMR studies of internal rotation and structural information from solid-state NMR, plus a full structure determination from powder x-ray diffraction in one case

2003 ◽  
Vol 41 (5) ◽  
pp. 324-336 ◽  
Author(s):  
Helen E. Birkett ◽  
Julian C. Cherryman ◽  
A. Margaret Chippendale ◽  
John S. O. Evans ◽  
Robin K. Harris ◽  
...  
Keyword(s):  
Solid State ◽  
Internal Rotation ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Structural Information ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
Structural Investigations ◽  
X Ray ◽  
Full Structure

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.

Solid-state NMR and X-ray diffraction structural investigations of the p-nitroaniline/ZSM-5 complex

2000 ◽  
Vol 39 (1-2) ◽  
pp. 291-305 ◽  
Author(s):  
Colin A Fyfe ◽  
Darren H Brouwer
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
Structural Investigations ◽  
X Ray

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

X-ray Diffraction and13C Solid-State NMR Studies of the Dimethylformamide Solvate of Tetra(C-undecyl)calix[4]resorcinarene

2000 ◽  
Vol 104 (9) ◽  
pp. 1921-1926 ◽  
Author(s):  
Marek Pietraszkiewicz ◽  
Oksana Pietraszkiewicz ◽  
Waclaw Kolodziejski ◽  
Krzysztof Wozniak ◽  
Neil Feeder ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray

Tetra(alkynyl)silanes, a 3,6-Disila-triyne, a 3,6,9-Trisila-tetrayne, a 1,3,4,6-Tetrasiladiyne, and Bis(trimethylstannyl)ethyne. Molecular Structures and Solid-state NMR Studies

2010 ◽  
Vol 65 (2) ◽  
pp. 119-127 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Ezzat Khan ◽  
Amin Badshah ◽  
Elias Molla ◽  
Peter Thoma ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Mas Nmr ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Solution State ◽  
Nmr Data

The molecular structures of three alkynylsilanes, tetrakis(ethynyl-p-tolyl)silane, 3,3,6,6,-tetramethyl- 3,6-disila-triyne, 3,3,6,6,9,9,-hexamethyl-3,6,9-trisila-tetrayne, and of bis(trimethylstannyl)- ethyne have been determined by X-ray diffraction. The same alkynylsilanes, and in addition 1,2- bis(trimethylsilylethynyl)-1,1,2,2-tetramethyldisliane, were studied by solid-state 13C and 29Si MAS NMR spectroscopy. The results of these measurements were compared with crystallographic evidence and also with relevant solution-state NMR data.

X-ray Diffraction and Solid-State NMR Studies of a Germanium Binuclear Complex

2006 ◽  
Vol 12 (2) ◽  
pp. 363-375 ◽  
Author(s):  
Luís Mafra ◽  
Filipe A. Almeida Paz ◽  
Fa-Nian Shi ◽  
João Rocha ◽  
Tito Trindade ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Binuclear Complex ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray

scholarly journals Exploiting the synergy of powder X-ray diffraction and solid-state NMR spectroscopy in a powerful strategy for structure determination of organic materials

2013 ◽  
Vol 69 (a1) ◽  
pp. s549-s549
Author(s):  
Dmytro Dudenko ◽  
P. Andrew Williams ◽  
Colan E. Hughes ◽  
Oleg N. Antzutkin ◽  
Sitaram P. Velaga ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Solid State Nmr ◽  
Organic Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy ◽  
Powerful Strategy

A simple molecule with a complex crystal structure: interplay of31P solid-state NMR spectroscopy and single-crystal x-ray diffraction in the structure determination of a ruthenium diphosphine diamine complex

2004 ◽  
Vol 42 (9) ◽  
pp. 807-813 ◽  
Author(s):  
Klaus Eichele ◽  
Christiane Nachtigal ◽  
Susanne Jung ◽  
Hermann A. Mayer ◽  
Ekkehard Lindner ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Complex Crystal Structure ◽  
Complex Crystal

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.

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