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Related Concept Videos

Determination of Crystal Structures01:29

Determination of Crystal Structures

In the late 1800s, the revelation that light extended beyond visible wavelengths led to the discovery of X-rays by Wilhelm Roentgen. Recognized as high-energy electromagnetic radiation with short wavelengths, X-rays prompted exploration into their interaction with crystals. Max von Laue proposed in 1912 that the periodic arrangement of atoms, ions, or molecules in crystals would cause them to diffract X-rays, a hypothesis confirmed through experiments with copper sulfate and zinc sulfide...
2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
Crystal Field Theory - Octahedral Complexes02:58

Crystal Field Theory - Octahedral Complexes

Crystal Field Theory
To explain the observed behavior of transition metal complexes (such as colors), a model involving electrostatic interactions between the electrons from the ligands and the electrons in the unhybridized d orbitals of the central metal atom has been developed. This electrostatic model is crystal field theory (CFT). It helps to understand, interpret, and predict the colors, magnetic behavior, and some structures of coordination compounds of transition metals.
CFT focuses on...
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied first.
Crystal Field Theory - Tetrahedral and Square Planar Complexes02:46

Crystal Field Theory - Tetrahedral and Square Planar Complexes

Tetrahedral Complexes
Crystal field theory (CFT) is applicable to molecules in geometries other than octahedral. In octahedral complexes, the lobes of the dx2−y2 and dz2 orbitals point directly at the ligands. For tetrahedral complexes, the d orbitals remain in place, but with only four ligands located between the axes. None of the orbitals points directly at the tetrahedral ligands. However, the dx2−y2 and dz2 orbitals (along the Cartesian axes) overlap with the ligands less than the dxy,...
2D NMR: Overview of Heteronuclear Correlation Techniques01:18

2D NMR: Overview of Heteronuclear Correlation Techniques

Heteronuclear correlation spectroscopy is an analytical technique that investigates the coupling between different types of nuclei, often a proton and an X-nucleus, such as carbon-13 or nitrogen-15. This method is commonly used in nuclear magnetic resonance (NMR) spectroscopy to gain insights into complex chemical compounds' structural and compositional aspects. A typical heteronuclear correlation spectrum displays X-nucleus chemical shifts on one axis and a proton spectrum on the other axis.

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Updated: Jun 21, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

Crystallographic structure refinement with quadrupolar nuclei: a combined solid-state NMR and GIPAW DFT example using

Cory M Widdifield1, David L Bryce

  • 1Department of Chemistry and Centre for Catalysis Research and Innovation, University of Ottawa, Ontario, Canada.

Physical Chemistry Chemical Physics : PCCP
|August 13, 2009
PubMed
Summary

Solid-state NMR and DFT calculations precisely measure bromine and magnesium properties. These methods reveal subtle solid-state structural details missed by X-ray diffraction.

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Fully Autonomous Characterization and Data Collection from Crystals of Biological Macromolecules
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Last Updated: Jun 21, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
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Fully Autonomous Characterization and Data Collection from Crystals of Biological Macromolecules
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Published on: March 22, 2019

Area of Science:

  • Solid-state chemistry
  • Materials science
  • Nuclear Magnetic Resonance (NMR) spectroscopy

Background:

  • Solid-state structure characterization is crucial for understanding material properties.
  • Powder X-ray diffraction (pXRD) is a common technique but has limitations in detecting subtle structural variations.
  • Nuclear Quadrupolar Coupling (NQC) is sensitive to local electronic environments.

Purpose of the Study:

  • To investigate the sensitivity of quadrupolar coupling constants for (79/81)Br and (25)Mg nuclei.
  • To explore the utility of solid-state NMR and GIPAW DFT in detecting subtle solid-state structural differences.
  • To compare the capabilities of NMR/DFT with pXRD for structural analysis.

Main Methods:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy was employed to measure quadrupolar coupling constants.
  • Generalized Inside-Out Projection-based Augmented Wave (GIPAW) Density Functional Theory (DFT) calculations were performed.
  • Results were compared with data obtained from powder X-ray diffraction (pXRD).

Main Results:

  • Both (79/81)Br and (25)Mg quadrupolar coupling constants demonstrated high sensitivity to minor changes in solid-state structure.
  • These NMR/DFT-derived parameters identified structural variations not discernible by pXRD.
  • The study highlights the power of combining experimental NMR with theoretical DFT for detailed structural elucidation.

Conclusions:

  • Solid-state NMR spectroscopy coupled with GIPAW DFT calculations offers enhanced sensitivity for detecting subtle structural features in solids.
  • This approach provides complementary information to pXRD, enabling a more comprehensive understanding of material structures.
  • The findings underscore the importance of advanced spectroscopic and computational techniques in materials characterization.