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Separating, correlating, and exploiting anisotropic lineshapes for NMR structure determination in solids

Walder, Brennan J
http://rave.ohiolink.edu/etdc/view?acc_num=osu1429846088

Abstract Details

2015, Doctor of Philosophy, Ohio State University, Chemical Physics.
Resolution and sensitivity in nuclear magnetic resonance (NMR) can be improved by eliminating the anisotropic influences from the spectrum, but this destroys useful information about the sample. Described in this thesis are methodological advances for enhancing the sensitivity and resolution of solid-state NMR in experiments that correlate or separate the anisotropic interactions. The symmetry pathway formalism is used to describe the invention of a new 2D correlation experiment called the shifting d-echo. It is twice as sensitive and more resistant to spectral artifacts than similar experiments in its class. The resolution exceeds that of experiments that do not correlate interactions. The capabilities of the shifting d-echo experiment are demonstrated by experiments probing the local structure, bonding, and magnetic properties of the iron group chloride dideuterates. The accuracy of the shifting d-echo measurements leads to a refined point-dipole model of the paramagnetic shift tensor in which the positions of the dipole sources are not restricted to the nuclei. Another new technique called Phase Incremented Echo Train Acquisition (PIETA) is introduced for enhancing the sensitivity of inhomogeneously broadened NMR spectra. With PIETA one can ensure coherence pathway selection over an entire train of echoes and collect information on the behavior of NMR interactions that are not refocused by the echo train. The ability of PIETA to enhance the sensitivity of a specific class of experiments designed to separate and correlate the information present in spinning sidebands is described extensively. The document concludes with a brief demonstration of how ideas behind phase cycling and symmetry pathways can be used to understand proton line narrowing magic echo train experiments. Pursuing this understanding has led to the invention of a new experiment for ensuring artifact free signal in magic echo train acquisition.
Philip Grandinetti, Prof. (Advisor)
Christopher Jaroniec, Prof. (Committee Member)
Ezekiel Johnston-Halperin, Prof. (Committee Member)
159 p.
Physical Chemistry
magnetic resonance, paramagnetic NMR, frequency anisotropy, nuclear quadrupolar coupling, Hahn echo, solid echo, magic echo, symmetry pathways, 2D NMR, point dipole model, NMR crystallography, spinning sidebands, PASS, MAT, PIETA, CPMG, TOP processing

Recommended Citations

Citations

  • Walder, B. J. (2015). Separating, correlating, and exploiting anisotropic lineshapes for NMR structure determination in solids [Doctoral dissertation, Ohio State University]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=osu1429846088

    APA Style (7th edition)

  • Walder, Brennan. Separating, correlating, and exploiting anisotropic lineshapes for NMR structure determination in solids. 2015. Ohio State University, Doctoral dissertation. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=osu1429846088.

    MLA Style (8th edition)

  • Walder, Brennan. "Separating, correlating, and exploiting anisotropic lineshapes for NMR structure determination in solids." Doctoral dissertation, Ohio State University, 2015. http://rave.ohiolink.edu/etdc/view?acc_num=osu1429846088

    Chicago Manual of Style (17th edition)

osu1429846088
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© 2015, all rights reserved.
This open access ETD is published by The Ohio State University and OhioLINK.