In Situ X-ray Diffraction and Solid-State NMR Study of the Fluorination of γ-Al2O3with HCF2Cl

2001 ◽  
Vol 123 (8) ◽  
pp. 1694-1702 ◽  
Author(s):  
Peter J. Chupas ◽  
Michael F. Ciraolo ◽  
Jonathan C. Hanson ◽  
Clare P. Grey
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Study

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.

Solid-State NMR, X-Ray Diffraction, and Theoretical Studies of Neutral Mononuclear Molecular Bis(triphenylphosphine)silver(I) Mono-Carboxylate and -Nitrate Systems

2020 ◽  
Vol 73 (6) ◽  
pp. 556
Author(s):  
Simon Grabowsky ◽  
Allan H. White ◽  
Peter C. Healy ◽  
Kim M. Lapere ◽  
Seik Weng Ng ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Crystal Packing ◽  
Computational Modelling ◽  
Inverse Correlation ◽  
X Ray Diffraction ◽  
Weakly Bound ◽  
X Ray ◽  
Nmr Study ◽  
Structure Determinations

Neutral mononuclear molecular silver(i) carboxylate complexes of the form [(Ph3P)2Ag(O2XY)] with O2XY=O2CCH2Ph, O2CCHPh2, O2CC(CH3)3, O2CCH2C(CH3)3, and O2CCF3 (compounds 1–4 and 5β) have been investigated in the solid state using single-crystal X-ray structure determinations, 1D 31P CPMAS NMR and 2D 31P–31P CPCOSY NMR measurements, and ab initio computational modelling. The results show that these complexes contain P2AgO2 molecular cores with four-coordinate silver in which the carboxylate ligands are weakly bound to the silver atoms via the two oxygen atoms giving rise to unsymmetrical chelate units. Crystal structure determinations and solid-state NMR spectra have also been analysed for the mononuclear molecular silver(i) nitrate complex [(Ph3P)2Ag(O2NO)] (9α) and two polymorphs of its toluene monosolvate (11α, β). In 9α, the two PPh3 ligands are of the same chirality, whereas in 11α, β, they are opposed. The crystalline environments in the polymorphs have been explored by way of Hirshfeld surface analyses, after quantum-mechanical isolated-molecule calculations had shown that although the molecular energies of the experimental geometries of 9α, and 11α, β are significantly different from each other and from the energies of the optimized geometries, the latter, in contrast, do not differ significantly from each other despite the conformational isomerism. It has further been shown using 9α as an example that the energy dependence on variation of the P–Ag–P angle over a range of ~15° is only ~5 kJ mol−1. All this indicates that the forces arising from crystal packing result in significant perturbations in the experimental geometries, but do not alter the stereoisomerism caused by the donor atom array around the Ag atom. In the NMR study, a strong inverse correlation has been found between 1J(107/109Ag,31P) and the Ag–P bond length across all carboxylate and nitrate compounds.

Phase Transformations in Porous Materials Studied by In Situ Solid-State NMR Spectroscopy and In Situ X-ray Diffraction

2020 ◽  
Vol 124 (35) ◽  
pp. 19136-19145
Author(s):  
Carolin Paula ◽  
Dorothea Wisser ◽  
Mojca Rangus ◽  
Wilhelm Schwieger ◽  
Maximilian Hovestadt ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Phase Transformations ◽  
Porous Materials ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Nmr Spectroscopy

Effect of melamine polyphosphate on thermal degradation of polyamides: a combined X-ray diffraction and solid-state NMR study

Polymer ◽  
2003 ◽  
Vol 44 (1) ◽  
pp. 25-37 ◽  
Author(s):  
Shahab Jahromi ◽  
Wouter Gabriëlse ◽  
Ad Braam
Keyword(s):  
Solid State ◽  
Thermal Degradation ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Study

Tautomerism in Schiff bases derived from 3-hydroxysalicylaldehyde. Combined X-ray diffraction, solution and solid state NMR study

2000 ◽  
pp. 935-939 ◽  
Author(s):  
Helene Pizzala ◽  
Micheline Carles ◽  
William E. E. Stone ◽  
Andre Thevand
Keyword(s):  
Solid State ◽  
Schiff Bases ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Study

In Situ Characterization of Waters of Hydration in a Variable-Hydrate Active Pharmaceutical Ingredient Using 35Cl Solid-State NMR and X-ray Diffraction

2019 ◽  
Vol 19 (12) ◽  
pp. 7349-7362 ◽  
Author(s):  
David A. Hirsh ◽  
Sean T. Holmes ◽  
Paroma Chakravarty ◽  
Austin A. Peach ◽  
Antonio G. DiPasquale ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
Active Pharmaceutical Ingredient ◽  
X Ray Diffraction ◽  
In Situ Characterization ◽  
X Ray

Mechanochemical Preparation of Hydrogen-Bonded Adducts Between the Diamine 1,4-Diazabicyclo[2.2.2]octane and Dicarboxylic Acids of Variable Chain Length: An X-ray Diffraction and Solid-State NMR Study

2003 ◽  
Vol 9 (22) ◽  
pp. 5538-5548 ◽  
Author(s):  
Dario Braga ◽  
Lucia Maini ◽  
Giorgiana de Sanctis ◽  
Katia Rubini ◽  
Fabrizia Grepioni ◽  
...  
Keyword(s):  
Solid State ◽  
Chain Length ◽  
Solid State Nmr ◽  
Dicarboxylic Acids ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Study ◽  
Hydrogen Bonded

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

Tautomeric polymorphism in salicylideneamine derivatives: an X-ray diffraction and solid-state NMR study

2000 ◽  
Vol 526 (1-3) ◽  
pp. 261-268 ◽  
Author(s):  
H. Pizzala ◽  
M. Carles ◽  
W.E.E. Stone ◽  
A. Thevand
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nmr Study

Structure and dynamics of condensed multivalent ions within polyelectrolyte bundles: a combined x-ray diffraction and solid-state NMR study

2005 ◽  
Vol 17 (14) ◽  
pp. S1123-S1135 ◽  
Author(s):  
Thomas E Angelini ◽  
Lori K Sanders ◽  
Hongjun Liang ◽  
Willy Wriggers ◽  
Jay X Tang ◽  
...  
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure And Dynamics ◽  
Multivalent Ions ◽  
Nmr Study
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