Dipsi2etgpjcsix1, Sensitivity and Gradient- enhanced HETLOC

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Warning: show this to your NMR facility manager before attempting to set up this experiment on your own!!!

Name: dipsi2etgpjcsix1
Platform: Bruker

Main article

Setting up

• power levels pl1 (for hard proton pulses) and pl2 (hard carbon pulses) will be specific to your instrument
• p1 at power pl1; calibrate pulse length p1 as ¹H 90^o pulse at power level pl1
• p6 at power pl10; set p6 for desired bandwidth of dipsi2 sequence, calculate pl10 so that p6 corresponds to ¹H 90^o pulse
• cnst2 - set to ¹J_CH (i.e. expected value of one-bond CH scalar couplings) in Hz
• cnst16 - scaling factor for ¹J_CH in indirect dimension. Default = 1. Set it so that multiplets of interest would not overlap in the final spectrum
• p3 @ pl2; calibrate p3 as ¹³C (or other X nucleus) 90^o pulse at power level pl2
• p14 @ sp3; typically p14 = 500 μs. Check value of spnam3 parameter. Calibrate power sp3 relative to pl2 and p2 so that shaped pulse spnam3 of length p14 corresponds to 180^{o 13}C inversion pulse. Calibration procedure will depend on the value of spnam3, i.e. nature of the shaped pulse.
• set o1p at the center of ¹H spectral window
• set o2p at the center of ¹³C chemical shift range to be affected by pulses p3 and p14
• type 'eda' and set spectral window of indirect ¹H proton dimension (SW parameter in the second column)
• set number of increments in the indirect dimension inside the 'eda' window so that you obtain desired value of digital resolution in that dimension
• at this time you can try typing gs then acqu and see how first fid looks like
• if the vertical span of fid does not fit into the screen - adjust rg parameter until it does
• adjust d1 and aq parameters so that you get acceptable length of recorded fid and sufficiently long relaxation between scans

Processing

NMRPipe data conversion script

#!/bin/csh

bruk2pipe -in ./ser  \
 -bad 0.0 -noaswap -DMX -decim 48 -dspfvs 12 -grpdly 0  \
 -xN              6400  -yN               490  \
 -xT              3173  -yT               245  \
 -xMODE            DQD  -yMODE        Echo-AntiEcho \
 -xSW         3968.254  -ySW         3967.073  \
 -xOBS         500.222  -yOBS         500.222  \
 -xCAR           4.773  -yCAR           4.773  \
 -xLAB             1Hx  -yLAB             1Hy  \
 -ndim               2  -aq2D          States  \
 -out ./test.fid -verb -ov

sleep 5

NMRPipe processing script

#!/bin/csh
nmrPipe    -in test.fid \
| nmrPipe  -fn SP -off 0.5 -end 1.00 -pow 2 -c 1.0             \
| nmrPipe  -fn ZF -size 16384                                   \
| nmrPipe  -fn FT                                               \
| nmrPipe  -fn PS -p0 -138.0 -p1 -14.2 -di                      \
| nmrPipe  -fn TP                                               \
| nmrPipe  -fn SP -off 0.5 -end 1.00 -pow 2 -c 0.5             \
| nmrPipe  -fn ZF -size 1024                                    \
| nmrPipe  -fn FT                                               \
| nmrPipe  -fn REV \
| nmrPipe  -fn PS -p0 94.0 -p1 -7.0 -di                         \
| nmrPipe  -fn TP                                               \
| nmrPipe -fn NULL -out test.DAT -verb 2 -ov