This two-dimensional phase-sensitive INADEQUATE experiment correlates
directly-bonded carbons. Before setting up the INADEQUATE experiment,
see Acquiring and Processing 2D Experiments. See the Varian
Guide to NMR Experiments for a complete description of this
experiment.
Sample Requirements: To obtain reasonable results within
24 hours, a 1-pulse 13C spectrum with nt=1 should
present a signal/noise ratio of at least 25:1 (position the cursors
in an empty region of the 1D spectrum and type dsn).
Acquiring the experiment:
1. Join the experiment in which the 13C reference spectrum was collected. Type inadqt.
2. Type dg. Adjust the parameters listed below for the standard INADEQUATE:
sfrq=100.559 dn=H1 dm='n'
tn=C13 dof = tof from 1H reference spectrum
at = set by spectrometer dm='y'
np=2048 dmm='w'
sw = sw from 13C reference spectrum dmf=9900
ss=2 dpwr=30
tpwr = listed at console sw1 = sw from 1H reference spectrm
pw = 13C 90° pulse width ni = multiple of 64
d1 = 1H relaxation delay (1-2 * 1H T1) dp='n'
d2=0 hs='yn'
presat='n' hst=0.01
phase=1,2 jcc=40
tof = tof from 13C reference spectrum rf1 = rf from 1H reference spectrum
nt = multiple of 4, maximum of 64 rfp1 = rfp from 1H reference spectrum
ct = set by computer wp1 = wp from 1H reference spectrum
sp1 = sp from 1H reference spectrum
Change ni, nt, and d1 to suit your scheduled time. The vertical (non-acquisition) resolution equals sw1/2ni. Typical values are listed below for sw1=25000:
d1 | ni | nt | time | vert. res | d1 | ni | nt | time | vert. res |
1.5 | 128 | 32 | 3:32 | 195 Hz |
1.5 | 128 | 128 | 14:10 | 195 Hz |
1.5 | 256 | 32 | 7:06 | 98 | 1.5 | 256 | 128 | 28:22 | 98 |
1.5 | 512 | 32 | 14:14 | 49 | 1.5 | 512 | 128 | 56:55 | 49 |
Processing, Displaying, and Plotting:
Process using the procedure for Processing a 2D Phase-Sensitive Experiment. Plot Pos. only contours.