lecture9_2006_jrl - Today’s Lecture 9) Wed, Oct 6:...

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Unformatted text preview: Today’s Lecture 9) Wed, Oct 6: Interactions of NMR in Solution and Solids a. Chemical shift b. J-coupling c. Dipole-dipole interactions d. Quadrupolar interactions e. Solid state NMR experimental considerations Review articles on ssNMR: • Angewandte Chemie 41 :3096-3129 (2002) • Accounts of Chemical Research 36 :858-865 (2003) • Current Opinion in Structural Biology 12 :661-669 (2002) Timescale Degrees of Freedom Magnetic Resonance Technique 3 2 1 ~0 Liquid NMR HRMAS Solid State NMR Determining the Technique Chemical shift Electrons surrounding a nucleus create a magnetic field (“shield”) which affects the size of the magnetic field seen at the nucleus Levitt Random Coil Carbon and Proton Shifts of Amino Acids Chemical Shift Referencing - +- = 2 1 cos 3 3 4 ) 1 ( 2 θ πχ σ V z H B π γ σ ν 2 / B 29- (1 = To compare shifts in liquids and solids, one must have a common referencing scheme. Can measure accurately Can not measure very accurately Would love to measure. Chemical Shifts depend on…everything •Temperature •Solvent •Concentration •Physical State •Conformation •Isotope effect MeOH CHCl 3 H 2 O NEAT TMS 2.0 1.0 0.0-1.0-2.0 DMSO Solvent Effects on TMS The 13 C TMS resonance is sensitive to solvent. Data shown at 600 MHz, under MAS, unlocked External Reference Zilm and Morcombe,“Chemical Shift Referencing in MAS Solid-State NMR,” J. Mag. Res. 2003 , 162 ,173. Chemical shift Electrons surrounding a nucleus create a magnetic field (“shield”) which affects the size of the magnetic field seen at the nucleus Levitt Molecules with different orientations will experience different induced fields.Molecules with different orientations will experience different induced fields....
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This note was uploaded on 06/07/2011 for the course BCH 6745 taught by Professor Staff during the Spring '08 term at University of Florida.

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lecture9_2006_jrl - Today’s Lecture 9) Wed, Oct 6:...

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