K. H. M. Jonsson, R. Pendrill and G. Widmalm
The 1DLR experiment devised by Nishida et al.[5] was used to References
3
measure the JC1 ,H2
ꢁ
coupling constant by a 13C site-selective
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1
The delay used for suppression of JC,H was set to (145 Hz)−1
and the time of the delay between excitation and coherence
transfer, for evolution of the long-range coupling, was set to 16
or 54 ms. When time-shared continuous-wave decoupling was
applied to the H1 resonance during acquisition the duty cycle
was 0.2. The two gradient pulses flanking the last pair of 90◦
pulses had their amplitudes set to 42.4 and 21.3 G cm−1, with
durations of 1 and 0.25 ms, respectively, and were followed by
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acquisition. A spectral width of 12 ppm was sampled with 34 962
data points using 745–6 k transients and an acquisition time of
2.1 s. Prior to Fourier transformation, zero-filling to 512 k data
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The 13C,1H-HETCOR experiment[29] was recorded with 64 scans
per t1-increment and a BIRD pulse to suppress the homonuclear
couplings in F1. A 2D matrix of 256 × 34 962 data points in
the F1 and F2 dimensions, respectively, was recorded with an
acquisition time of 1.0 s. Prior to Fourier transformation zero-filling
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sine-bell functions were applied in both dimensions. The 1H,13C-
HSQC-HECADE experiment[38] was recorded with 192 scans per
t1-increment, a DIPSI-2 spin-lock and a mixing time of 30 ms. A
2D matrix of 256 × 2 k data points in the F1 and F2 dimensions,
respectively, a t1∗/t1 scaling factor of unity and the echo/anti-echo
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foldlow-passJ-filter(J = 140, 155and170 Hz)tosuppressthe1JC,H
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to be measured, were used to scale the coupling in the indirect (F1)
dimension. The measurements were performed with seven scaling
factorsbetween15and18forthe2JC,H couplingconstantsandfour
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Experiments were performed with 512 × 2 k data points in the F1
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with the echo/anti-echo method. Spectral width was 6 ppm in 1H
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2
and in 13C it was 100 ppm for the experiments measuring JC,H
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3JC,H. Prior to Fourier transformation of all J-HMBC experiments
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90◦ shifted sine-bell window function multiplication. Coupling
constants were extracted from 1D projections of the resonances
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This work was supported by grants from the Swedish Research
Council,TheKnutandAliceWallenbergFoundation,TheLarsHierta
Memorial Foundation and Carl Tryggers Stiftelse fo¨r Vetenskaplig
Forskning. The Swedish NMR Centre at Go¨teborg University is
thanked for access to a high field spectrometer.
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c
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Magn. Reson. Chem. 2011, 49, 117–124