lecture9_2006_jrl - Today's Lecture 9 Wed Oct 6...

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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)
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Timescale Degrees of Freedom Magnetic Resonance Technique 3 2 1 ~0 Liquid NMR HRMAS Solid State NMR Determining the Technique
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Chemical shift Electrons surrounding a nucleus create a magnetic field (“shield”) which affects the size of the magnetic field seen at the nucleus Levitt
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Random Coil Carbon and Proton Shifts of Amino Acids
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Chemical Shift Referencing - + - = 2 1 cos 3 3 4 ) 1 ( 2 0 θ πχ σ V z H B π γ σ ν 2 / 0 B 29 - (1 = To compare shifts in liquids and solids, one must have a common referencing scheme. Can measure accurately Can not measurevery accurately Would loveto measure. Chemical Shifts depend on…everything •Temperature •Solvent •Concentration •Physical State •Conformation •Isotope effect
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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.
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Chemical shift Electrons surrounding a nucleus create a magnetic field (“shield”) which affects the size of the magnetic field seen at the nucleus Levitt
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Molecules with different orientations will experience different induced fields.
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