Bruker BioSpin Solid State NMR, User Manual

Page: 312 / 328

312 (327) BRUKER BIOSPIN User Manual Version 002
Figures
13 SUPER 169
Figure 13.1. Pulse Sequence for 2D CPMAS exchange experiment........................................... 170
Figure 13.2. The “123” Icon in the Menu Bar of the Data Windows Acquisition Parameter Page. 171
Figure 13.3. The Acquisition Parameter Window (eda) .............................................................. 172
Figure 13.4. The SUPER Spectrum of Tyrosine HCl After Processing Using “xfb” ...................... 175
Figure 13.5. SUPER spectrum after tilting the spectrum setting “1 alpha” = -1 ........................... 176
Figure 13.6. Various Cross Sections from the Upper 2D Experiment ......................................... 177
14 Symmetry Based Recoupling 179
Figure 14.1. C7 SQ-DQ Correlation Experiment ........................................................................ 181
Figure 14.2. Optimization of the RF power level for DQ generation/reconversion on glycine. ..... 184
Figure 14.3. Variation of DQ-generation/reconversion time on a uniformly 13C labeled peptide (fM-
LF). ....................................................................................................................... 184
Figure 14.4. PC7 Recoupling Efficiency at a Spinning Speed of 13 kHz ..................................... 185
Figure 14.5. SC14 2d SQ-DQ correlation on tyrosine-HCl ......................................................... 189
Figure 14.6. PC7 2d SQ-SQ correlation on tyrosine-HCl ........................................................... 191
15 PISEMA 193
Figure 15.1. Pisema Pulse Sequence ....................................................................................... 194
Figure 15.2. PISEMA Spectrum of 15N Labeled Acetylated Valine and FID in t1 over 3.008 ms 64
Data Points ........................................................................................................... 199
Figure 15.3. PISEMA Spectrum of 15N Labeled Kdpf Transmembrane Protein. ......................... 200
16 Relaxation Measurements 201
Figure 16.1. The CPX T1 Pulse Sequence ................................................................................ 203
Figure 16.2. Relaxation of Alpha-carbon Signal in Glycine ........................................................ 207
17 Basic MQ-MAS 213
Figure 17.1. A 3-Pulse Basic Sequence with Z-Filter. ................................................................ 214
Figure 17.2. A 4-Pulse Basic Sequence with Z-Filter. ................................................................ 214
Figure 17.3. Comparison of 87Rb MAS spectra of RbNO3 excited with selective and non-selective
pulses. .................................................................................................................. 217
Figure 17.4. Nutation profiles of selective and non-selective pulses. ......................................... 218
Figure 17.5. Example for popt Set-up for Optimization of p1 and p2. ......................................... 219
Figure 17.6. Signal Intensities of 87Rb Resonances in RbNO3 as Function of p1 and p2........... 220
Figure 17.7. 2D 87Rb 3QMAS Spectrum of RbNO3. .................................................................. 223
Figure 17.8. Comparison of Differently Processed 2D 23Na 3Q MAS Spectra of Na4P2O7. ....... 224
Figure 17.9. Calculated Shift Positions dMQ ............................................................................. 225
Figure 17.10. 17O MQMAS of NaPO3 at 11.7 T (67.8 MHz) on the left and 18.8 T (108.4 MHz) on the
right. ..................................................................................................................... 228
Figure 17.11. Slices and Simulations of the 18.8 T 17O MQMAS of NaPO3. .............................. 229
Figure 17.12. Graphical Interpretation of the Spectrum from
Figure 17.10.
. ............................... 230
18 MQ-MAS: Sensitivity Enhancement 231
Figure 18.1. Hahn Echo Pulse Sequence and Coherence Transfer Pathway. ............................. 232
Figure 18.2. Processing of Hahn Echo. Left is the Shifted Echo. ............................................... 233
Figure 18.3. Four Pulse Sequence and Coherence Transfer Pathway for the 3Q MAS Experiment ..
234
Figure 18.4. Three Pulse Sequence and Coherence Transfer Pathway ...................................... 234