scholarly journals Single-Crystal X-ray and Solid-State NMR Characterisation of AND-1184 and Its Hydrochloride Form

Materials ◽  
2021 ◽  
Vol 14 (23) ◽  
pp. 7175
Author(s):  
Tomasz Pawlak ◽  
Małgorzata Szczesio ◽  
Marek J. Potrzebowski
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Quantum Chemical ◽  
Structural Investigation ◽  
Monoclinic Crystal ◽  
Rigid System ◽  
X Ray ◽  
Dynamic Motion ◽  
Nmr Study

In this study, we report on a structural investigation of AND-1184, with the chemical name N-[3-[4-(6-fluoro-1,2-benzoxazol-3-yl)piperidin-1-yl]propyl]-3-methylbenzenesulfonamide (MBS), and its hydrochloride form (MBSHCl); AND-1184 is a potential API for the treatment of dementia. The single-crystal X-ray investigation of both forms results in monoclinic crystal systems with P21/c and C2/c symmetry for MBS and MBSHCl, respectively. This solid-state NMR study, combined with quantum-chemical calculations, allowed us to assign all 13C and most 1H signals. The MBS structure was defined as a completely rigid system without significant dynamic behaviours, whereas MBSHCl exhibited limited dynamic motion of the aromatic part of the molecule.

Substituent and Solvent Effects on Intermolecular Interactions in Crystals of N-Acylhydrazone Derivatives: Single-Crystal X-ray, Solid-State NMR, and Computational Studies

2014 ◽  
Vol 14 (5) ◽  
pp. 2263-2281 ◽  
Author(s):  
Liliana Mazur ◽  
Katarzyna N. Jarzembska ◽  
Radosław Kamiński ◽  
Krzysztof Woźniak ◽  
Edyta Pindelska ◽  
...  
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Intermolecular Interactions ◽  
Solvent Effects ◽  
Solid State Nmr ◽  
Computational Studies ◽  
X Ray

scholarly journals A combined single crystal neutron/X-ray diffraction and solid-state nuclear magnetic resonance study of the hybrid perovskites CH3NH3PbX3 (X = I, Br and Cl)

2015 ◽  
Vol 3 (17) ◽  
pp. 9298-9307 ◽  
Author(s):  
Tom Baikie ◽  
Nathan S. Barrow ◽  
Yanan Fang ◽  
Philip J. Keenan ◽  
Peter R. Slater ◽  
...  
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Single Crystal ◽  
Solid State Nmr ◽  
Variable Temperature ◽  
Neutron Diffraction Study ◽  
Nuclear Magnetic Resonance Study ◽  
X Ray Diffraction ◽  
Magnetic Resonance Study ◽  
X Ray

This article describes a variable temperature solid-state NMR and single crystal X-ray/neutron diffraction study of the hybrid perovskites (CH3NH3)PbX3 (X = I, Br and Cl).

Structural investigation of SnO–B2O3 glasses by solid-state NMR and X-ray photoelectron spectroscopy

2002 ◽  
Vol 306 (3) ◽  
pp. 227-237 ◽  
Author(s):  
Akitoshi Hayashi ◽  
Miyuki Nakai ◽  
Masahiro Tatsumisago ◽  
Tsutomu Minami ◽  
Yusuke Himei ◽  
...  
Keyword(s):  
Solid State ◽  
Photoelectron Spectroscopy ◽  
Solid State Nmr ◽  
Structural Investigation ◽  
X Ray

Metal polypyrazolylborates XIII. Solution and solid state NMR study of cyano—mercury(II) polypyrazolylborates. X-ray crystal structure of [HB(3,5-Me2pz)3]HgCN

1997 ◽  
Vol 539 (1-2) ◽  
pp. 9-17 ◽  
Author(s):  
Giancarlo Gioia Lobbia ◽  
Patrizio Cecchi ◽  
Roberto Gobetto ◽  
Giuseppe Digilio ◽  
Riccardo Spagna ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Solid State Nmr ◽  
X Ray ◽  
Nmr Study

ChemInform Abstract: Hydrogen Bonding and the Structure of Substituted Quinoxalines: Solid- State NMR and Single-Crystal X-Ray Diffraction Studies.

ChemInform ◽  
2010 ◽  
Vol 24 (25) ◽  
pp. no-no
Author(s):  
K. WOZNIAK ◽  
T. M. KRYGOWSKI ◽  
E. GRECH ◽  
W. KOLODZIEJSKI ◽  
J. KLINOWSKI
Keyword(s):  
Hydrogen Bonding ◽  
Solid State ◽  
Single Crystal ◽  
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.

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