Structure determination of aligned systems by solid-state NMR magic angle spinning methods

The X-ray crystal structure determination of bis[-(phenylcyanamido)bis(triphenylphosphine)copper(I)], [{Cu(PPh3)2(C6H5NCN)}2], (1) is reported. The complex has a centrosymmetric dimeric structure with the phenylcyanamide ligands bridging the copper atoms in a -1,3-fashion. The structure is compared with that of the 4-methylphenylcyanamido complex, [{Cu(PPh3)2(4-MeC6H4NCN)}2] (2), and the differences observed in the Cu–P bond lengths compared with changes in the solid state 31P cross-polarization magic-angle spinning (CPMAS) spectra of the two complexes.

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Filamentous Bacteriophage Viruses: Preparation, Magic-Angle Spinning Solid-State NMR Experiments, and Structure Determination

Methods in Molecular Biology - Protein NMR ◽

10.1007/978-1-4939-7386-6_4 ◽

2017 ◽

pp. 67-97 ◽

Cited By ~ 4

Author(s):

Omry Morag ◽

Nikolaos G. Sgourakis ◽

Gili Abramov ◽

Amir Goldbourt

Keyword(s):

Solid State ◽

Structure Determination ◽

Solid State Nmr ◽

Magic Angle Spinning ◽

Magic Angle ◽

Filamentous Bacteriophage ◽

Angle Spinning

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Dihedral Angle Measurements for Structure Determination by Biomolecular Solid-State NMR Spectroscopy

Frontiers in Molecular Biosciences ◽

10.3389/fmolb.2021.791090 ◽

2021 ◽

Vol 8 ◽

Author(s):

Patrick C. A. van der Wel

Keyword(s):

Solid State ◽

Structure Determination ◽

Solid State Nmr ◽

Structural Information ◽

Magic Angle Spinning ◽

Magic Angle ◽

Distance Measurements ◽

Challenges And Opportunities ◽

Molecule Interactions ◽

Angle Spinning

In structural studies of immobilized, aggregated and self-assembled biomolecules, solid-state NMR (ssNMR) spectroscopy can provide valuable high-resolution structural information. Among the structural restraints provided by magic angle spinning (MAS) ssNMR the canonical focus is on inter-atomic distance measurements. In the current review, we examine the utility of ssNMR measurements of angular constraints, as a complement to distance-based structure determination. The focus is on direct measurements of angular restraints via the judicious recoupling of multiple anisotropic ssNMR parameters, such as dipolar couplings and chemical shift anisotropies. Recent applications are highlighted, with a focus on studies of nanocrystalline polypeptides, aggregated peptides and proteins, receptor-substrate interactions, and small molecule interactions with amyloid protein fibrils. The review also examines considerations of when and where ssNMR torsion angle experiments are (most) effective, and discusses challenges and opportunities for future applications.

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Determination of Phase Content in Multiphase Polymers by Solid-State NMR Techniques

Materials Science Forum ◽

10.4028/www.scientific.net/msf.714.51 ◽

2012 ◽

Vol 714 ◽

pp. 51-56 ◽

Cited By ~ 2

Author(s):

Antonio Martínez-Richa ◽

Regan Silvestri

Keyword(s):

Solid State ◽

Solid State Nmr ◽

Magic Angle Spinning ◽

Polymer Chains ◽

Magic Angle ◽

Aliphatic Polyesters ◽

Polymer Systems ◽

Nmr Techniques ◽

Angle Spinning

Solid-state nuclear magnetic resonance (NMR) spectroscopy has emerged as a relatively facile technique for the characterization of multi-component polymer systems. In particular, it has emerged to be a useful technique for probing the molecular structure, conformation and dynamics of polymer chains at interfaces between phases in various types of multi-component polymer systems including nanomaterials. The usefulness of solid-state NMR stems from its ability to non-destructively probe not only the bulk of the polymer, but moreover its ability to selectively probe the interface or interphase. As such, the technique has been extensively exploited in the study of multi-component polymer systems. To achieve13C spectral resolution in the solid-state magic angle spinning (MAS), dipolar decoupling and cross-polarization are applied which enables the study of individual carbon atoms directly with excellent resolution and sensitivity. Some examples of applications of this technique to the study of multiphase aliphatic polyesters are reviewed herein.

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