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Solid State Nuclear Magnetic Resonance Studies Of ~D 6447 LBNL-42160 ~RNE55T ~lFUANIDC’2 b3A/W?ENK3E Gafmfm a’=-!- 51ERKELXY NIA-T-UEHWQL bd3C3RATClHFW’ Solid-StateNuclearMagnetic ,,,>,, ., -. .-..-... “,,-z,,’>.J ResonanceStudiesof CrossPolarizationlkom QuadrupolarNuclei .- SusanM. De Paul ,. Materials Sciences Division August 1997 . Ph.D. Thesis -. ,.... ,. 0 .. : . .,,,.- ,. ,. .?... ‘I.. ‘.,,.. ---- -... .,. r, .“ ““ . .,.. ,, .,. DISCLAIMER This document was prepared as an account of work sponsored by the United Statea Government. While this document is believed to contain correct information, neither the United States Government nor any agency thereof, nor The Regents of the University of California, nor any of their employees, makes any warranty, express or implied, or assumes any legaf responsibility for the accuracy, completeness, or usefulness of ~Y information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by its trade name, trademmk, manufacturer, or otherwise, does not necessarily constitute or impIy its endorsement, recommendation, or favoring by the United States Government or arty agency thereof, or The Regents of the University of Cafifomia. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof, or The Regents of the University of Cafifomia. Ernest Orlando Lawrence Berkeley NationaI Laboratory is an equaI opportunity employer. DISCLAIMER Portions of this document may be iilegibfe in electronic image products. Images are produced from the best avaiiable original document. !., , . - . --,,-q- --.<. -. - ;--- -- . ~ . - .-G.. LBNL-42160 Solid-State Nuclear Magnetic Resonance Studies of Cross Polarization from Quadrupolar Nuclei Susan Margaret De Paul Ph.D. Thesis Department of Chemistry University of California, Berkeley and Materials Sciences Division Ernest Orlando Lawrence Berkeley National Laboratory University of California Berkeley, CA 94720 August 1997 This workwas supportedby the Dkector,Officeof EnergyResearch,OffIceof BasicEnergySciences, MaterialsSciencesDivision,of the U.S.Departmentof EnergyunderContractNo. DE-AC03-76SFOO098. .7. ,.J . - .,. ...:! , ,-,. ,:->.. ..,, ., c’ i~.. ..,- ,-’.’.J - ,.”’, . Solid-State Nuclear Magnetic Resonance Studies of Cross Polarization from Quadrupolar Nuclei by Susan Margaret De Paul A.B. (Harvard University) 1992 A dissertation submitted in partial satisfaction of the requirements for the degree of Doctor of Philosophy in Chemistry in the GRADUATE DIVISION of the UNIVERSITY of CALIFORNIA, BERKELEY Committee in charge: Professor Alexander Pines, Chair Professor A. Paul Alivisatos Professor Alexis T. Bell Fall 1997 .- .;.- . ,. Solid-State Nuclear Magnetic Resonance Studies of Cross Polarization from Quadrupolar Nuclei Copyright 01997 by Susan Margaret De Paul The U.S. Departmentof Energyhas the right to use this document for any purposewhatsoeverincludingthe right to reproduce all or anypart thereof .. ,...>- .-r, ,7,...:. ,.:., ..- .<- . r.-,,.-,-,-,-,.:,--. ,-- -- Abstract Solid-State Nuclear Magnetic Resonance Studies of Cross Polarization from Quadrupolar Nuclei by Susan Margaret De Paul Doctor of Philosophy in Chemistry University of California, Berkeley Professor Alexander Pines, Chair The development of solid-state Nuclear Magnetic Resonance (NMR) has, to a large extent, focused on using spin-1/2 nuclei as probes to investigate molecular structure and dynamics. For such nuclei, the technique of cross polarization is well-established as a method for sensitivity enhancement. However, over two-thirds of the nuclei in the periodic table have a spin-quantum number greater than one-half and are known as quadrupolar nuclei. Such nuclei are fundamental constituents of many inorganic materials including minerals, zeolites, glasses, and gels. It is, therefore, of interest to explore the extent to which polarization can be transferred from quadrupolar nuclei. In this dissertation, solid-state NMR experiments involving cross polarization from quadrupolar nuclei to spin-1/2 nuclei under magic-angle spinning (MAS) conditions are investigated in detail. The behavior of the central transition of a quadrupolar nucleus under a low-power radiofrequency spin-lock field is examined both experimentally and with numerical simulations. Complications in choosing the matching spin-lock field strength for the spin- 1/2 nucleus are discussed. The dynamics of the cross-polarization process are characterized in a model compound (low albite) and a protocol for optimizing the polarization-transfer efficiency is presented. Significant enhancement of 29Si NMR sensitivity by using 27A1-to-29Si and 23Na-to-29Si cross polarization is demonstrated in several inorganic compounds. This sensitivity enhancement permits otherwise impractical two-dimensional NMR experiments to be performed. Cross polarization from quadrupolar nuclei is incorporated into experiments designed to correlate the isotropic and anisotropic parts of the chemical-shielding tensor. Several different pulse sequences for performing such 1 ,< ,,. ~,>.., ., ‘f.. ,.. .’.:.’. ,., ‘S’.,.,-:. .—— 2 correlations under magic-angle spinning conditions are analyzed and compared. Cross polarization from quadrupokir nuclei ‘is also ‘;ombined with the recently-developed Multiple-Quantum Magic-Angle Spinning (MQMAS) experiment to create a new technique for measuring heteronuclear correlation spectra. In addition, the motion of cyclopentadienyl rings in four organometallic solids is studied by variable-temperature NMR, and two-dimensional exchange spectroscopy is used to demonstrate that sigmatropic rearrangements occur in the monohaptocyclopentadienyl groups of Hf(q5-C5H5)2(q *-C5H5)2. An experiment which “ demonstrates that a rapid mechanical sample reorientation leads to a time reversal of radio-frequency driven spin diffusion among 13C spins is also presented. For my parents iv ,. .,,.,,. .—f,-. - ~...,., ,: ., .,.,:. Table of Contents 1 Introduction . ..*...... 1 1.1 Quantum Fundamentals . .- . ..--- . ...-..1 1.1.1 Density Matrix . ...2 1.1.2 Interaction Representation . .--.....6 1.1.3 Wigner Rotation Matrices . - . ...10 1.1.4 Perturbation Theory . ...-.13 1.2 NMRHamiltonians . ...14 1.2.1 Spin Operators andthe ZeemanInteraction . ..14 1.2.2 RfIrradiation, RotatingFrame, and BlochEquations . ...16 1.2.3 Chemical-Shielding Interaction. - . ...18 1.2.4 Dipolar Interaction . ...21 1.2.5 Quadrupolar Interaction . -- . - . ..-....22 1.2.6 Other Interactions inner . ...31 1.3 Powder Spectra . ...32 1.4 Rotating Samples . ...33 1.4.1 Wigner Rotation Matrices Revisited. ...33 1.4.2 EffectsofSample Rotation onQuadmpolaf Lineshapes . ...37 1.5 Phase Cycling andDataProcessing . ...38 1.5.1 Coherence-TransferPathways.. ...39 1.5.2 Pure-Phase Two-Dimensional Spectra . ...43 2 13CVariab1e-Temperature CP/’MASStudies ofTetracyclopentadienyl Complexes . 51 2.1 Fluxional Motion in Organometallic Compounds . ...51 2.2 One-Dimensional ‘3CVariable-Temperature CP/MASExperiments . ...54 2.2.1 SnCp4 Spectra . ...58 2.2.2 HfCp4 Spectra . ...61 2.2.3 ZrCp4 Spectra . ...65 2.3 Two-dimensional Exchange Spectroscopy . 67 v \ . .. ,,, ,,:’ ~’:,, .,.. ,.,, ———.... 2.4 Comparison of HfCp4 and TiCp4 Exchange Spectra . ..75 3 Spin Locking of Quadrupolar Nuclei During MAS . 79 3.1 Low Albiteas aModelCompound. ...79 3.2 Spin Locking ofHalf-Integer QuadrupolarNuclei . ...83 3.3 Spin Loclcing intheSuddenRegime . ...89 3.4 Directmeasurement ofthe27Aland23Na Tlp’sinlowalbite . ...101 4 CrossPolarization ofQuadrupolarNuclei DuringMAS Using Low RadiofrequencyField Amplitudes . ...* . ..O.OO 103 4.1 Previous S~diesof Cross Pol.mization Involving Quadmpolar Nuclei . 103 4.2 Experimental Parameters . ..105 4.3 Hartmann-Hahn Matching for Quadrupolar Nuclei . .. 107 4.4 Cross-Polarization Dynamics for Quadrupolar Nuclei. ...11 6 4.5 Prognosis for Cross-Polarization from Quadrupolar Nuclei Using Low-Rf Field Strengths . .. ...131 5 Applications of Cross Polarization from Quadrupolar Nuclei to Aluminosilicates ● . 137 5.1 Isotropic-Anisotropic Correlation Spectroscopy . .‘. .137 5.2 Magic-Angle Hopping . ...138 5.3 Isotropic-Anisotropic Correlation by Slow Spinning. 139 5.3.1 Theory of Magic-Angle Turning Experiments. ...140 5.3.2 MATwith 90° Pulses . .145 5.3.3 MATwith 180° Pulses . ... .148 5.3.4 TOSS-reTOSS . ...151 5.4 Application of Isotropic-Anisotropic Correlation Methods to Low Albite . ...154 5.5 Experiments on Low Microcline . ..158 5.6 Validity of Using Cross Polarization from Quadrupolar Nuclei . ...159 5.7 REDORExperiments . ..161 6 High-Resolution Heteronuclear Correlation between Quadrupolar and Spin- 1/2 Nuclei using Multiple-Quantum Magic-Angle Spinning... ...166 6.1 Methods for Obtaining High-Resolution Spectra of Quadmpolm Nuclei . ...166 6.1.1 DOuble Rotation (DOR) . ...167 6.1.2 Dynamic-Angle Spinning (DAB) . ...169 6.1.3 Multiple-Quantum Magic-Angle Spinning (MQMAS) . ...173 6.2 Heteronuclem Conflation and Quadmpolar Nuclei . 180 6.2.1 MAS-and DAS-Based Techniques.. .180 6.2.2 MQMAS-HETCOR . ..183 7 Reversal ofRadiofrequency-Driven SpinDiffusionby Reorientationof the Sample-Spinning Axis . 194 7.1 Previous Polarization-Echo Experiments . ..194 7.2 Spin Diffusion . ...195 7.3 Reversal of Rf-Driven Spin Diffusion . ...198 7.3.1 Pulse Sequence and Experimental Apparatus . 198 7.3.2 Build-up of Cross-Peak Intensity . ...200 7.3.3 Spin-Diffusion Echoes . ...204 vii ...., .<, . .. .L”.
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