Guest dynamics and crystal structure of the tri-o-thymotide-acetone clathrate studied by solid-state NMR, X-ray diffraction and molecular modelling

1992 ◽  
Vol 5 (10) ◽  
pp. 670-682 ◽  
Author(s):  
G. A. Facey ◽  
C. I. Ratcliffe ◽  
R. Hynes ◽  
J. A. Ripmeester
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Molecular Modelling ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

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 Linear dicoordinate beryllium: a 9Be solid-state NMR study of a discrete zero-valent s-block beryllium complex

2018 ◽  
Vol 96 (7) ◽  
pp. 646-652 ◽  
Author(s):  
C. Leroy ◽  
J.K. Schuster ◽  
T. Schaefer ◽  
K. Müller-Buschbaum ◽  
H. Braunschweig ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Chemical Shift ◽  
Solid State Nmr ◽  
Chemical Shift Tensor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Quadrupolar Coupling ◽  
Nmr Study ◽  
Tensor Data

Beryllium-9 (9Be) quadrupolar coupling and chemical shift tensor data are reported for bis(1-(2,6-diisopropylphenyl)-3,3,5,5-tetramethylpyrrolidine-2-ylidene)beryllium (Be(CAAC)2). These are the first such data for beryllium in a linear dicoordinate environment. The 9Be quadrupolar coupling constant, 2.36(0.02) MHz, is the largest recorded in the solid state to date for this isotope. The span of the beryllium chemical shift tensor, 22(2) ppm, covers about half of the known 9Be chemical shift range, and the isotropic 9Be chemical shift, 32.0(0.3) ppm, is the largest reported in the solid state to our knowledge. DFT calculations reproduce the experimental data well. A natural localized molecular orbital approach has been used to explain the origins and orientation of the beryllium electric field gradient tensor. The single-crystal X-ray structure of a second polymorph of Be(CAAC)2 is also reported. Inspection of the powder X-ray diffraction data shows that the new crystal structure is part of the bulk product next to another crystalline phase. Therefore, experimental X-ray powder data for the microcrystalline powder sample and the SSNMR data do not fully match either the originally reported crystal structure (Arrowsmith et al. Nat. Chem. 2016, 8, 890–894) or the new polymorph. The ability of solid-state NMR and powder X-ray diffraction to characterize powdered samples was thus particularly useful in this work.

scholarly journals Crystal structure and guest motional behavior of Cd(CN)2cyclohexane clathrate. X-ray diffraction and solid-state NMR study

1996 ◽  
Vol 52 (a1) ◽  
pp. C292-C292
Author(s):  
S. Nishikiori ◽  
T. Kitazawa ◽  
C. I. Ratcliffe ◽  
J. A. Ripmeester ◽  
T. Iwamoto
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Study ◽  
Motional Behavior

Revisiting the crystal structure of dickite: X-ray diffraction, solid-state NMR, and DFT calculations study

2018 ◽  
Vol 103 (5) ◽  
pp. 812-818 ◽  
Author(s):  
João Rocha ◽  
Filipe A. Almeida Paz ◽  
Mariana Sardo ◽  
Luís Mafra
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Dft Calculations ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

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.

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.

High-temperature, high-pressure hydrothermal synthesis, crystal structure, and solid state NMR Spectroscopy of a lead borosilicate with boron-silicon mixing: Pb6B2Si8O25

2021 ◽  
Author(s):  
Ling-Wei Chang ◽  
Kwang-Hwa Lii
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
High Temperature ◽  
Hydrothermal Synthesis ◽  
Solid State ◽  
Solid State Nmr ◽  
Hydrothermal Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
High Temperature High Pressure

A new lead(II) borosilicate, Pb6B2Si8O25 (1), has been synthesized by a high-temperature, high-pressure hydrothermal reaction at 480 °C and 990 bar. Its structure was determined by single-crystal X-ray diffraction. The...

A MOF based on a lead(II) 2-oxido-6-methylpyridine-4-carboxylate network

2020 ◽  
Vol 75 (4) ◽  
pp. 365-369
Author(s):  
Long Tang ◽  
Yu Pei Fu ◽  
Na Cui ◽  
Ji Jiang Wang ◽  
Xiang Yang Hou ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Carboxylic Acid ◽  
Thermogravimetric Analysis ◽  
Metal Organic Framework ◽  
X Ray Diffraction ◽  
X Ray ◽  
Connected Node ◽  
Metal Organic ◽  
Solid State Fluorescence

AbstractA new metal-organic framework, [Pb(hmpcaH)2]n (1), has been hydrothermally synthesized from Pb(OAc)2 · 3H2O and 2-hydroxy-6-methylpyridine-4-carboxylic acid (hmpcaH2; 2), and characterized by IR spectroscopy, elemental and thermogravimetric analysis, and single-crystal X-ray diffraction. In complex 1, each hmpcaH− ligand represents a three-connected node to combine with the hexacoordinated Pb(II) ions, generating a 3D binodal (3,6)-connected ant network. The crystal structure of 2 was determined. The solid-state fluorescence properties of 1 and 2 were investigated.

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