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

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 Determination of a complex crystal structure in the absence of single crystals: analysis of powder X-ray diffraction data, guided by solid-state NMR and periodic DFT calculations, reveals a new 2′-deoxyguanosine structural motif

2017 ◽  
Vol 8 (5) ◽  
pp. 3971-3979 ◽  
Author(s):  
Colan E. Hughes ◽  
G. N. Manjunatha Reddy ◽  
Stefano Masiero ◽  
Steven P. Brown ◽  
P. Andrew Williams ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State Nmr ◽  
Structural Motif ◽  
X Ray Diffraction ◽  
X Ray ◽  
Complex Crystal Structure ◽  
Complex Crystal ◽  
Periodic Dft Calculations ◽  
Periodic Dft

A multi-technique strategy reveals a new hydrogen-bonding motif for a 2′-deoxyguanosine derivative.

Influence of fluorine side-group substitution on the crystal structure formation of benzene-1,3,5-trisamides

CrystEngComm ◽  
2014 ◽  
Vol 16 (39) ◽  
pp. 9273-9283 ◽  
Author(s):  
Christoph Zehe ◽  
Marko Schmidt ◽  
Renée Siegel ◽  
Klaus Kreger ◽  
Venita Daebel ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Structure Formation ◽  
Solid State Nmr ◽  
Quantum Chemical ◽  
Side Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Structure Formation

The crystal structure of 1,3,5-tris(2-fluoro-2-methylpropionylamino)benzene was solved by combining powder X-ray diffraction, solid-state NMR spectroscopy and quantum chemical calculations.

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.

Crystal structure of phenanthrenide salts stabilized by 15-crown-5 and 18-crown-6

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Natalie Eichstaedt ◽  
Kasper P. van der Zwan ◽  
Lina Mayr ◽  
Renée Siegel ◽  
Jürgen Senker ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Coordination Number ◽  
Solid State Nmr ◽  
Inert Atmosphere ◽  
Potassium Cation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solvent Molecules

Abstract Potassium 15-crown-5 phenanthrenide and potassium 18-crown-6 phenanthrenide were synthesized and characterized by powder X-ray diffraction and 39K solid state NMR spectroscopy. While the radical carbanion is very reactive in solution, the crystals are stable and storable under inert atmosphere. For 15-crown-5, a sandwich-like complex of potassium is formed with two molecules of crown ether per potassium resulting in a coordination number of 10. For the larger 18-crown-6 ligand, a 1:1 complex is obtained and a coordination number of 6 for the potassium cation. In neither crystal structure solvent molecules are incorporated. The 15-crown-5 compound crystallizes faster and is less soluble in THF as compared to the 18-crown-6 compound. Both compounds form solid phenanthrenide that is easy to handle and can be applied for reduction reactions.

A Coordination Polymer of Bis-[2-(dimethylamino)ethanolato]dimethylsilane with a Lithium Chloride Dimer

2009 ◽  
Vol 64 (3) ◽  
pp. 343-346
Author(s):  
Michael Hagemann ◽  
Tania Pape ◽  
Norbert W. Mitzel
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Coordination Polymer ◽  
Lithium Chloride ◽  
X Ray Diffraction ◽  
X Ray ◽  
Chloride Adduct

The reaction of lithium 2-(dimethylamino)ethanolate with Me2SiCl2 yielded a lithium chloride adduct of Me2Si- (OCH2CH2NMe2)2. Despite the application of an excess of Me2SiCl2, the formation of ClMe2SiOCH2CH2NMe2 was not observed. [Me2Si(OCH2CH2NMe2)2・Li2Cl2] was characterised by NMR spectroscopy and determination of its crystal structure by X-ray diffraction. In the solid state it forms endless chains consisting of Li2Cl2 rhombi, with the lithium atoms chelated by the O and N atom of one OCH2- CH2NMe2 substituent of Me2Si(OCH2CH2NMe2)2 units.

Model compounds of aromatic nylons. 3. The conformation of the 4T Nylon, poly(tetramethylene terephthalamide), using X-ray diffraction, solid-state 13C nmr spectroscopy and ir spectroscopy

1989 ◽  
Vol 67 (5) ◽  
pp. 840-849 ◽  
Author(s):  
Josée Brisson ◽  
Johanne Gagné ◽  
François Brisse
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Nmr Spectroscopy ◽  
Hydrogen Bonds ◽  
Solid State Nmr ◽  
13C Nmr Spectroscopy ◽  
X Ray Diffraction ◽  
Model Compounds ◽  
X Ray ◽  
Structure Determinations

Three model compounds of poly(tetramethylene terephthalamide) or 4T Nylon have been synthesized and characterized using single crystal X-ray diffractometry, infrared spectroscopy, and 13CCP/MAS nmr spectroscopy. The model compounds are the para-substituted N,N′-tetramethylene dibenzamides, where the substituents are the—OMe, —tBu, —CN, and —CH3 groups. The crystal structure determinations reveal three distinct conformations for the CO—NH—(CH2)4—NH—CO sequence of atoms. The conformation is all trans for OMe, tgtttg−t for the tBu substituent, and tsttts−t for the CN substituent ([Formula: see text], [Formula: see text], and [Formula: see text]). In all three derivatives, the dihedral angle between the aromatic ring and the amide plane is around 30°. The OMe and tBu para-substituted molecules are interconnected by nearly linear hydrogen bonds of normal N … O distances. However, for the CN derivative the N … O distance is exceptionally short, 2.402(4) Å. On the basis of its infrared and solid state nmr spectra, it is proposed that N,N′-tetramethylene di-para-methyl benzamide has a crystal structure comparable to that of its unsubstituted analog. The methylenic sequence of the parent polyamide, 4T Nylon, has the tgtttg−t conformation. Furthermore, the polyamide chains form sheets within which the chains, parallel to one another, are connected through hydrogen bonds. Keywords: polyamide, crystal structure, solid-state nmr.

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