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by: Adah McCullough III


Adah McCullough III
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Class Notes
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This 13 page Class Notes was uploaded by Adah McCullough III on Saturday September 12, 2015. The Class Notes belongs to BCMB 4190 at University of Georgia taught by Urbauer in Fall. Since its upload, it has received 63 views. For similar materials see /class/202190/bcmb-4190-university-of-georgia in Biochemistry and Molecular Biology at University of Georgia.

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Date Created: 09/12/15
CHEM BCMB 419061908189 Introductory NMR Lecture 15 Introduction to 2D NMR 1D NMR spectrum X axis is the directly detected frequency and y axis gives the intensity problem of overlap of the detected frequencies defining connections between spins using selective excitation may be impossible H H OCH 8 o 9 7 I H0 H HHO H 3 COOCH3 J H HN 3 Ac 5 OH H H 1 3a COOCH OCH CHAC 4amp5 H9 17 H3e HJn rv39v l l I 40 35 30 25 20 1H6ppm 2D NMR spectrum X and y are frequency axes and the intensity constitutes the z axis 39 39 25 5 0 00 o u u 3a5 E 5 9739 3a4 quot 3997 175 OCH32 e M 100 t 125 1150 O 3a1 SIQOCH 39 394To39 39 39 393T539 1 r 33 r 39 3925 39239o 1 3ppm 2D J resolved spectrum 39 X axis is the directly detected frequency 39 y axis is the coupling constant 39 resolves problems of overlap in 1D spectrum 2D shift correlated NMR spectrum 39 X and y are frequency axes 1H 1H 1H 13C 1H lsN etc 39 defines connections between nuclear spins 3D NMR spectrum 39 2D NMR is good for MW up to 1012 kD in studies of proteins more dimensions increased the resolution for studies of larger systems X y and z are frequency axes 39 the intensity constitutes the fourth dimension 39 for sensitivity reason 1H is usually the detected frequency 8 0 73 Connections hhWppn two quot H Throughbond correlation based of J coupling between nuclear dipoles gives information on the covalent structure torsion angle constraint Example COSY HETCOR TOCSY HSQC N Throughspace correlation based on dipolar interactions NOE nuclear Overhauser effect gives information on the geometrical structure distance constraint Example NOESY DJ Chemical exchange correlation based on dynamic processes gives info on these dynamic processes Example EXSY General Experimental Scheme In 1D NMR IPreparation I Acquisition PREPARATION period a single pulse in the most simple case and multiple pulses and delays in more complex pulse sequences Example J modulated spinecho experiment INEPT DEPT In 2D NMR Two new elements the EVOLUTION and MIXING periods are introduced between the preparation and the acquisition period The EVOLUTION period introduces an indirectlydetected frequency dimension During the MIXING period coherence is transferred from one spin to another IPreparation IEvolutiont1 Mixing IAcquisitiont2 In 3D NMR Combination of 2D NMR experiments lPreparation IEvoluti0nt1 Mixing lAcquisitiont2 2D lPreparation lEvolutiont1 Mixing lAcquisitiont2 2D Combine IPreparation lEvolutiont1 Mixing IEvolutiont2 Mixing IAcquisitiont8 3D General Scheme for TwoDimensional NMR selected 2D experiments detection t2 preparation evolution t1 COSY t1 NOESY t1 TOCSY t1 90x 180x 90 180 H Hr W r W Hch 180x 90 5 13C E COSY Correlated Spectroscopy NOESY Nuclear Overhauser Effect Spectroscopy TOCSY Total Correlation Spectroscopy HSQC Heteronuclear Single Quantum Correlation decouple Heteronuclear TwoDimensional IResolved NMR Spectroscopy A Pulse sequence Experiment similar to the J modulated spinecho pulsesequence The fixed delay 1 is now a variable delay t12 H WW WHB 15 WA 13C 90 180 H FL FID l an I k r12 ff 3 b c d B Vector diagram Lets consider a twospin AX system with A 1H and X 13C as in 13CHCl3 v 13CHaCl3 39Vc 12JCH v 13CHpC13 Vc 12JCH o 2nJCH t12 a b c d e MCHOL MCHOL MCHOL m l y39 r39 y 7 y39 McH W W chH KMcH McH 39 x39 x MchS x39 x x H 0 t1 12J t1 1J t1 32J t1 2J J coupling evolves during the first t12 delay only 0 Field inhomogeneity is refocused by the 180 y pulse 0 Chemical shift evolution in t1 is refocused by the 180 y39 pulse For simplicity ignore relaxation C Fourier transform in t2 We perform quot11quot experiments with various values of t1 and Fourier transform all quot11quot experiments t1 gt H 0 t1 12J t1 1J t1 32J t1 2J D Amplitude modulation in t1 t1 gt o 12J 1J 32J 2J o The amplitude is modulated in t1 at a frequency related to J CH E Second Fourier transform in t1 J1 J72 l J4 O J4 A second Fourier transform With respect to t1 yields two frequencies With a separation of J CW2 F Summary FT FT 8t1t2 gtSt1F2 gtSF1F2 F2 dimension contains the 13C chemical shift F1 dimension contains the coupling constant For 13CHCl3 39 The signal induced in the receiver depends on the sum of the two vectors which depends on JCH After FT of the FID with respect to t2 a single 13C signal is observed in the frequency spectrum F2 no splitting 39 The 13C signal is modulated by the value of JCH and the value of t1 After FT of the FID with respect to t1 a doublet centered at zero frequency is observed in the frequency spectrum F1 with a splitting of JCH 2 For more complex molecules 39 In F2 Cq CH CH2 and CH3 are all singlets 39 In F1 Cq singlet CH2 triplet CH doublet CH3 quartet G Choice of acquisition time in t1 39 Should be long enough to give satisfactory resolution in F1 Digital resolution 1 acquisition time in t1 39 Also limited by relaxation Graphical Representation Two forms of display are generally used Stacked plot a series of F2 spectra for different F1 values are plotted above one another Each trace is shifted by a constant amount relative to the preceding one For CHCI3 13C 6 777 ppm JCH 209 Hz L A L JL 7 3 50 F 7 F1 7 A 250 Hz J 7717 5 30 F 2 Contour plot the peaks are seen from above as in a topographic map The section is taken at certain height above the plane of the F1 and F2 axes and the contours at that level are plotted For CHCI3 13C 6 777 ppm JCH 209 Hz 0 50 F1 0 Hz 0 50 777 mt For more complex molecules CH CHJAd 2 l llll I l II Iquot I so hertz 39 1oo 150 l I l 39 110 100 90 80 70 60 50 L0 30 20 6 2 ppm 10 Other example of contour plots 2D 1HISN correlation spectrum HSQC plotted at various levels a z a z H ppm Eve 2 Eve 2 H ppm Eve 2 3w 2 11 Homonuclear TwoDimensional JResolved NMR Spectrosconv A Pulse sequence Experiment similar to the J modulated spinecho pulse sequence The xed delay 1 is now a variable delay t1 In homonuclear case not possible to use BB decoupling The 180X39 pulse is applied to both spins A and X 2 90 130 HO J IL Vv lt mz al I r2 f a o b c B Vector diagram Lets consider a homonuclear twospin AX system 39VA Xa 39VA 12JAX VA X5 39VA 12JAX 9 27cJAX t1 J coupling evolves during both t12 delays 0 Field inhomogeneity is refocused by the 180 X39 pulse MA I y W Xa X39 0 Chemical shift evolution in t1 is refocused by the 180 X39 pulse 0 For simplicity ignore relaxation 12 B Contour plot For a 1H AX svstem The signal induced in the receiver depends on the sum of the two vectors which depends on JAX After FT of the FID with respect to t2 two 1H peaks are observed These two peaks are tilted relative to F2 but the spectrum can be manipulated to bring all the component of the multiplet at the same F2 frequency no splitting The 1H signals are modulated by the value of JAX and the value of t1 After FT of the FID with respect to t1 a doublet centered at zero frequency is observed in the frequency spectrum F1 with a splitting of J AX JAX 10 Hz 10Hz O 5 F1 Spectral 0 5 F1 Manipulation quot 0 t H u 0 Hz Hz 0 5 o 5 61H 6 1H


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