35Cl solid-state NMR of HCl salts of active pharmaceutical ingredients: structural prediction, spectral fingerprinting and polymorph recognition

CrystEngComm ◽  
2014 ◽  
Vol 16 (31) ◽  
pp. 7334-7356 ◽  
Author(s):  
Marcel Hildebrand ◽  
Hiyam Hamaed ◽  
Andrew M. Namespetra ◽  
John M. Donohue ◽  
Riqiang Fu ◽  
...  
Keyword(s):  
Solid State ◽  
Plane Wave ◽  
Dft Calculations ◽  
First Principles ◽  
Solid State Nmr ◽  
Active Pharmaceutical Ingredients ◽  
Structural Prediction ◽  
Pharmaceutical Ingredients

A series of HCl salts of active pharmaceutical ingredients (APIs) have been characterized via35Cl solid-state NMR (SSNMR) spectroscopy and first-principles plane-wave DFT calculations of 35Cl NMR interaction tensors.

scholarly journals Combining solid-state NMR spectroscopy with first-principles calculations – a guide to NMR crystallography

2016 ◽  
Vol 52 (45) ◽  
pp. 7186-7204 ◽  
Author(s):  
Sharon E. Ashbrook ◽  
David McKay
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Dft Calculations ◽  
First Principles ◽  
Solid State Nmr ◽  
Nmr Spectra ◽  
First Principles Calculations ◽  
Recent Developments ◽  
Future Potential ◽  
Nmr Crystallography

DFT calculations are an important tool in assigning and interpreting NMR spectra of solids: we discuss recent developments and their future potential in the context of NMR crystallography.

scholarly journals Identifying the Molecular Edge Termination of Exfoliated Hexagonal Boron Nitride Nanosheets with Solid-State NMR Spectroscopy and Plane-Wave DFT Calculations

2019 ◽  
Author(s):  
Rick W. Dorn ◽  
Matthew J. Ryan ◽  
Tae-Hoon Kim ◽  
Tian Wei Goh ◽  
Patrick M. Heintz ◽  
...  
Keyword(s):  
Solid State ◽  
Boron Nitride ◽  
Plane Wave ◽  
Dft Calculations ◽  
Solid State Nmr ◽  
Hexagonal Boron Nitride ◽  
Magic Angle Spinning ◽  
Magic Angle ◽  
Edge Termination ◽  
Boron Nitride Nanosheets

Hexagonal boron nitride nanosheets (h-BNNS), the isoelectric analog to graphene, have received much attention over the past decade due to their high thermal oxidative resistance, high bandgap, catalytic activity and low cost. The molecular functional groups that terminate boron and nitrogen zigzag and/or armchair edges directly affect their chemical, physical and electronic properties. However, an understanding of the exact molecular edge termination present in h-BNNS is lacking. Here, high-resolution magic-angle spinning (MAS) solid-state NMR (SSNMR) spectroscopy and plane-wave density-functional theory (DFT) calculations are used to determine the exact molecular edge termination in exfoliated h-BNNS. 1H→11B cross-polarization MAS (CPMAS) SSNMR spectra of h-BNNS revealed multiple hydroxyl/oxygen coordinate boron edge sites that were not detectable in direct excitation experiments. A dynamic nuclear polarization (DNP)-enhanced 1H→15N CPMAS spectrum of h-BNNS displayed four distinct 15N resonances while a 2D 1H{14N} dipolar-HMQC spectrum revealed three distinct 14N environments. Plane-wave DFT calculations were used to construct model edge structures and predict the corresponding 11B, 14N and 15N SSNMR spectra. Comparison of the experimental and predicted SSNMR spectra confirms that zigzag and armchair edges with both amine and boron hydroxide/oxide termination are present. The detailed characterization of h-BNNS molecular edge termination will provide usefulness for many material science applications and the techniques outlined here should be applicable to comprehensively understand the molecular edge terminations in other 2D materials.

On the relaxation dynamics in active pharmaceutical ingredients: solid-state 1H NMR, quasi-elastic neutron scattering and periodic DFT study of acebutolol hydrochloride

RSC Advances ◽  
2015 ◽  
Vol 5 (71) ◽  
pp. 57502-57514 ◽  
Author(s):  
A. Pajzderska ◽  
K. Drużbicki ◽  
A. Kiwilsza ◽  
M. A. Gonzalez ◽  
M. Jarek ◽  
...  
Keyword(s):  
Molecular Dynamics ◽  
Solid State ◽  
Dft Calculations ◽  
Neutron Scattering ◽  
Active Pharmaceutical Ingredients ◽  
Relaxation Dynamics ◽  
Elastic Neutron ◽  
Pharmaceutical Ingredients ◽  
Elastic Neutron Scattering ◽  
Periodic Dft

Molecular dynamics of acebutolol hydrochloride was thoroughly explored by combining QENS and NMR experiments with solid-state DFT calculations.

scholarly journals Ab initio 35Cl solid state NMR-based crystallography of active pharmaceutical ingredients

2016 ◽  
Vol 72 (a1) ◽  
pp. s117-s117
Author(s):  
Angeles Pulido ◽  
David A. Hirsh ◽  
Robert W. Schurko ◽  
Graeme M. Day
Keyword(s):  
Solid State ◽  
Ab Initio ◽  
Solid State Nmr ◽  
Active Pharmaceutical Ingredients ◽  
Pharmaceutical Ingredients

DNP-enhanced solid-state NMR spectroscopy of active pharmaceutical ingredients

2018 ◽  
Vol 56 (7) ◽  
pp. 583-609 ◽  
Author(s):  
Li Zhao ◽  
Arthur C. Pinon ◽  
Lyndon Emsley ◽  
Aaron J. Rossini
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Solid State Nmr ◽  
Active Pharmaceutical Ingredients ◽  
Solid State Nmr Spectroscopy ◽  
Pharmaceutical Ingredients

Chemical shift reference scale for Li solid state NMR derived by first-principles DFT calculations

2018 ◽  
Vol 297 ◽  
pp. 33-41 ◽  
Author(s):  
S.S. Köcher ◽  
P.P.M. Schleker ◽  
M.F. Graf ◽  
R.-A. Eichel ◽  
K. Reuter ◽  
...  
Keyword(s):  
Solid State ◽  
Chemical Shift ◽  
Dft Calculations ◽  
First Principles ◽  
Solid State Nmr ◽  
Reference Scale

scholarly journals Structural Study of La1–xYxScO3, Combining Neutron Diffraction, Solid-State NMR, and First-Principles DFT Calculations

2013 ◽  
Vol 117 (5) ◽  
pp. 2252-2265 ◽  
Author(s):  
Karen E. Johnston ◽  
Martin R. Mitchell ◽  
Frédéric Blanc ◽  
Philip Lightfoot ◽  
Sharon E. Ashbrook
Keyword(s):  
Solid State ◽  
Neutron Diffraction ◽  
Dft Calculations ◽  
Structural Study ◽  
First Principles ◽  
Solid State Nmr
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