Read-Me instructions for pulse program ASAP-HSQC (14/02/28)

Important Note !!!
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The ASAP-HSQC is an experiment utilizing a high repetition rate and a high duty cycle. THIS MAY DAMAGE YOUR PROBEHEAD! Use it on your own risk and/or ask your spectrometer supplier. Make sure that the probe head is suitable for the high duty cycle, in case you are uncertain choose a higher value for the recovery delay d1.

Disclaimer: The  pulse program has been tested and used on a Bruker AVANCE III 600 MHz spectrometer equipped with a 1H,13C,15N TCI cryoprobe at the Karlsruhe Institute of Technology (KIT). The sequence is made available without any expressed warranty. We are not liable for any potential damage that might be caused in connection with the pulse program. We are not responsible for any damage on your hardware or software caused by the use of this pulse program.



Folder contents
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dataset:	example data set for menthol in CDCl3 
pulse files: 	shaped pulse files that have to be copied as described below. 
pulse program:	pulse program that has to be copied as described below. 





Experimental Details: Shaped Pulses, TOCSY, Ernst angle
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The pulse program should be copied into the folder:

"Your Topspin folder"/exp/lists/pp/user
(e.g.:  /opt/topspin3.2/exp/lists/pp/user)


The pulse program uses shaped pulses on both channels (1H and 13C). Corresponding shape files are attached. References to the shaped pulses can be found at the end of this instruction. To get started, you have to copy the pulse shape files into the following folder of your spectrometer computer:

"Your Topspin folder"/exp/lists/wave/user
(e.g.:  /opt/topspin3.2/exp/lists/wave/user)

The spectrometer should then automatically recognize the pulse shapes. Note that \ instead of / has to be used on Windows-PCs.

All shaped pulses with the given pulse lengths are defined with rf-amplitudes of 20kHz (1H) and 10kHz(13C). Therefore the power levels of the shaped pulses have to be calibrated by a 90° hard pulse with a duration of 12.5 us for 1H , and 25 us for 13C, respectively.

The delay d9 defines roughly the TOCSY mixing time. In the provided dataset it is adjusted to 30 ms, corresponding to a real mixing time of 34.53 ms. This value yielded best result for the utilized sample menthol but other values might be better for different samples.

The initial, optimized transfer delay (defined by cnst3) in the INEPT step can be seen as an equivalent to the Ernst-angle excitation scheme. For best results, It should be optimized for every sample individually. To our experience, a value of cnst3=210 Hz should provide good results for most small molecules.



Please write difficulties or experiences to:

Burkhard.Luy@kit.edu

Positive comments are also welcome!

Reference of the pulse sequence:
D. Schulze-Sünninghausen , J. Becker , and B. Luy, J. Am. Chem. Soc., 2014, 136 (4), pp 1242–1245

References of the used pulses:
Kobzar, K.; Skinner, T.; Khaneja, N.; Glaser, S.; Luy, B. J. Magn. Reson. 2004, 170, 236-243.
Kobzar, K.; Skinner, T. E.; Khaneja, N.; Glaser, S. J.; Luy, B. J. Magn. Reson. 2008, 194, 58-66.
Skinner, T.; Kobzar, K.; Luy, B.; Bendall, M.; Bermel, W.; Khaneja, N.; Glaser, S. J. Magn. Reson. 2006, 179, 241-249.
Skinner, T.; Reiss, T.; Luy, B.; Khaneja, N.; Glaser, S. J. Magn. Reson. 2003, 163, 8-15.
Skinner, T.; Reiss, T.; Luy, B.; Khaneja, N.; Glaser, S. J. Magn. Reson. 2004, 167, 68-74.
Kobzar, K.; Ehni, S.; Skinner, T. E.; Glaser, S. J.; Luy, B. J. Magn. Reson. 2012, 225, 142-160.
Ehni, S.; Luy, B. Magn. Reson. Chem. 2012, 50, S63-S72; (b) Ehni, S.; Luy, B. J. Magn. Reson. 2013, 232, 7-17.
Luy, B.; Kobzar, K.; Skinner, T.; Khaneja, N.; Glaser, S. J. Magn. Reson. 2005, 176, 179-186.
Skinner, T. E.; Gershenzon, N. I.; Nimbalkar, M.; Bermel, W.; Luy, B.; Glaser, S. J. J. Magn. Reson. 2012, 216, 78-87.