Protocol: optimal sampling of relaxation

Setup

Python installation

Required libraries:

• numpy
• scipy
• matplotlib
• numba
• json

Setting up python scripts

Ensure #! in analyse_results.py and final_results.py points to the correct python interpreter.

Set field strength in response_surface.py.

Setting up bruker bits

Copy files from bruker-bits into python script directory:

cp run_adaptive_methyl_ccr.py /opt/topspin/exp/stan/nmr/py/user/
cp -r simplejson /opt/topspin/exp/stan/nmr/py/user/

Edit run_adaptive_methyl_ccr.py to set appropriate experiment names and directories (at top of script file)

Setup pulse sequence

Use sequence adaptive_hsqcphpr.cw:

acquisition parameters:

• o1p = 0.7 ppm
• cnst21 = (bf hz) for off-resonance pre-sat
• d0 = 13C evolution time (compensating for 13C 90 pulses) > 20 us
• phcor7 = detection phase
• o2p = 11 ppm
• aq = 100 ms, td = 4k
• d1 = 1 s

processing parameters:

• WDW = EM
• LB = 5 Hz
• COROFFS = cnst21 - o1 (i.e. put solvent suppression on-resonance with water)
• BCmod = qfil
• SI = 16k
• set phase correction based on run with d0=20us and phcor7=0

Chemical shifts

Measure using HMQC:

Peak: 1H shift: -0.2573 0.1958 0.4057 0.65367 0.7437 13C shift: 10.4281 11.3917 10.9918 10.784 11.8283

Optional debugging flags

od/optimal_design.py: PLOT = True

Running

run_adaptive_methyl_ccr

• monitor output directory for result files
• don't let anyone use the computer during acquisition!

To interrupt acquisition:

• create a file named 'STOP' in the main experiment directory: touch STOP

Analysing results

Use script final_results.py:

• Pass the experiment directory (containing adapt_ccr_* files) as a command line argument
• Set the number of seed points at the top of the script file (for plotting)