The selective 1D INADEQUATE (SELINQUATE) experiment is
the selective version of the 1D INADEQUATE
experiment. This experiment allows to measure carbon-carbon coupling
constants and to assign 13C-13C connectivities.
REQUIREMENTS
Easy implementation on AVANCE spectrometers with selective
excitation using shaped pulses. However, the signals due to 13C-13C
couplings are 1/200 the intensity of the signal from a single 13C.
For this reason, the INADEQUATE experiment has a very low sensitivity and
high sample concentrations are usually required
VERSIONS
The selective ge-1D INADEQUATE pulse sequence can easily derived
of the 1D INADEQUATE pulse
sequence by converting the last 13C pulse of the sequence selective
for a selected 13C resonance
(
88ANG1196
). The sequence is based on the creaction of
homonuclear multiple-quantum coherences.
Similar modified approaches have been reported:
Using a DANTE pulse train
(
96CONC119
)
as a selective excitation scheme.
Improved sensitivity by using multiple-selective excitation
(
92MRC1247
and
93JMRA42-102
).
Selective version using a heteronuclear-chemical-shift-filter to measure
1J(CC)
(
87MRC798
and
92MRC68
).
It has also been used to measure nJ(CC)
(
91MRC561
).
Improved results can be obtained from gradient-enhanced experiments as,
for instance, the GRECCO experiment.
A related selective 1D 13C COSY experiment has also been applied
to 13C-labeled compounds
(
90MRC149
).
EXPERIMENTAL DETAILS
The selective 1D INADEQUATE experiment can be run with minor
changes from a predefined parameter set. Detailed description of the experiment
can be found in the original publication
(
86JMR106-70
).
Two important parameters to consider are:
Selectivity of the selective excitation pulse:
the user must define the shape, the duration and the power level needed
for a defined excitation profile.
Optimization of the J-coupling evolution delay
as a function of 1/(2*J(CC)), in order to get the anti-phase magnetization
of the selected carbon suitable for transfer polarization.
For further details on practical implementation of selective 1D INADEQUATE
experiments on AVANCE spectrometers see Tutorial: selective 1D INADEQUATE
experiment.
SPECTRA
The selective INADEQUATE spectrum only shows the 13C
nuclei directly and/or long-range J-coupled to the selected 13C
nucleus. These signals appear as anti-phase doublets from which 1J(CC)
and nJ(CC) can be measured.
RELATED TOPICS
An excellent review describing selective excitation in 1D and
multidimensional NMR experiments was published
(
91MRC527
).