skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Low Temperature Solid-State NMR Spectroscopy. A Strategy for the Direct Observation of Quadrupolar Nuclides of Biological Interest.

Abstract

This review presents a self-contained summary of the experimental methods necessary to perform a low temperature solid-state NMR experiment. Specific references are made for Zn²⁺ and Mg²⁺. However, this is not a comprehensive review of the NMR literature of these nuclides. As the review is concerned with solid-state NMR spectroscopy of quadrupolar nuclides, we limit the discussions to odd-half-integral spin systems, i.e. 3/2, 5/2, 7/2, and 9/2 spins. The reason for the limitation is due to the “relative ease” of observing the central transition, which is common to all of these nuclides. The review is divided into two major sections; the first dealing with experimental methods, e.g. use of low temperature, magnetization transfer, spin echo methods, and questions dealing with nonspecific binding. Following those discussions we turn to the introduction of structure into the experiment, i.e. the use triple resonance experiments to selectively introduce dipolar interactions and the use of molecular theory.

Authors:
;
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
917216
Report Number(s):
PNWD-SA-6612
TRN: US200816%%348
DOE Contract Number:
AC05-76RL01830
Resource Type:
Book
Resource Relation:
Related Information: Annual Reports on NMR Spectroscopy, 60:1-38
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; NUCLEAR MAGNETIC RESONANCE; ZINC; MAGNESIUM; SPIN ECHO; MAGNETIZATION

Citation Formats

Ellis, Paul D., and Lipton, Andrew S. Low Temperature Solid-State NMR Spectroscopy. A Strategy for the Direct Observation of Quadrupolar Nuclides of Biological Interest.. United States: N. p., 2007. Web.
Ellis, Paul D., & Lipton, Andrew S. Low Temperature Solid-State NMR Spectroscopy. A Strategy for the Direct Observation of Quadrupolar Nuclides of Biological Interest.. United States.
Ellis, Paul D., and Lipton, Andrew S. Mon . "Low Temperature Solid-State NMR Spectroscopy. A Strategy for the Direct Observation of Quadrupolar Nuclides of Biological Interest.". United States. doi:.
@article{osti_917216,
title = {Low Temperature Solid-State NMR Spectroscopy. A Strategy for the Direct Observation of Quadrupolar Nuclides of Biological Interest.},
author = {Ellis, Paul D. and Lipton, Andrew S.},
abstractNote = {This review presents a self-contained summary of the experimental methods necessary to perform a low temperature solid-state NMR experiment. Specific references are made for Zn²⁺ and Mg²⁺. However, this is not a comprehensive review of the NMR literature of these nuclides. As the review is concerned with solid-state NMR spectroscopy of quadrupolar nuclides, we limit the discussions to odd-half-integral spin systems, i.e. 3/2, 5/2, 7/2, and 9/2 spins. The reason for the limitation is due to the “relative ease” of observing the central transition, which is common to all of these nuclides. The review is divided into two major sections; the first dealing with experimental methods, e.g. use of low temperature, magnetization transfer, spin echo methods, and questions dealing with nonspecific binding. Following those discussions we turn to the introduction of structure into the experiment, i.e. the use triple resonance experiments to selectively introduce dipolar interactions and the use of molecular theory.},
doi = {},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Mon Jan 01 00:00:00 EST 2007},
month = {Mon Jan 01 00:00:00 EST 2007}
}

Book:
Other availability
Please see Document Availability for additional information on obtaining the full-text document. Library patrons may search WorldCat to identify libraries that hold this book.

Save / Share:
  • Metal ions play an important role in bioinorganic chemistry, however, following their respective chemistries is often complicated because several relevant metal ions (such as V5+, Cu1+, Zn2+, and Mg2+) are not always amenable to conventional UV/Vis or EPR spectroscopy. Rather, what we know of these metal sites has come from the characterization of the various compounds and proteins via x-ray crystallographic methods or from using surrogate metal probes for conventional spectroscopy
  • Solid-state NMR spectroscopy of half-integer quadrupolar metals has received a lot of interest recently with the advent of new methodologies and higher magnetic fields. We present here the extension of our previous low temperature method to an 18.8 T system. This new probe entailed a total redesign including a cross coil and variable capacitors that are operational at cryogenic temperatures. The limitations to sensitivity are also discussed; including a new diode network, the utilization of a cryogenic band pass filter, and the consequences of the RF profiles of the coil. Further, details of the spectroscopy of a spin 5/2 metalmore » in a protein are discussed, such as the observation of the outer transitions and how to distinguish them from the desired {+-}1/2 transition« less
  • Proteins directly control the nucleation and growth of biominerals, but the details of molecular recognition at the protein-biomineral interface remain poorly understood. The elucidation of recognition mechanisms at this interface may provide design principles for advanced materials development in medical and ceramic composites technologies. Here, we describe both the theory and practice of double-quantum solid-stateNMR(ssNMR) structure-determination techniques, as they are used to determine the secondary structures of surface-adsorbed peptides and proteins. In particular, we have used ssNMR dipolar techniques to provide the first high-resolution structural and dynamic characterization of a hydrated biomineralization protein, salivary statherin, adsorbed to its biologically relevantmore » hydroxyapatite (HAP) surface. Here, we also review NMR data on peptides designed to adsorb from aqueous solutions onto highly porous hydrophobic surfaces with specific helical secondary structures. The adsorption or covalent attachment of biological macromolecules onto polymer materials to improve their biocompatibility has been pursued using a variety of approaches, but key to understanding their efficacy is the verification of the structure and dynamics of the immobilized biomolecules using double-quantum ssNMR spectroscopy.« less
  • The quadrupolar and chemical shift tensors, as well as the relative orientation of the two principle axis systems, are accurately determined using a two-dimensional nuclear magnetic resonance technique. Good agreement between experimental and simulated two-dimensional spectra is obtained for a series of rubidium and sodium compounds at multiple magnetic field strengths. Extension of this technique to correlate the quadrupolar and dipolar interactions, as well as the incorporation of a purely isotropic dimension resulting in a three-dimensional experiment is also discussed. {copyright} {ital 1996 American Institute of Physics.}