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Assignment of proton signals was achieved through two-dimensional (2D) experiments: homonuclear 1H-1H correlation spectroscopy (COSY), total correlation spectroscopy (TOCSY), nuclear Overhauser enhancement spectroscopy (NOESY), and heteronuclear 1H-13C heteronuclear single-quantum correlation (HSQC), and heteronuclear multiple bond coherence (HMBC).
CH5 H41/42 cross-peaks in NOESY spectra differentiated C from U in the TOCSY spectra and initiated assignment of proton resonances.
For the complete assignment of proton and carbon signals, 1D (H, homodecoupled H [22], C and DEPT-135) as well as 2D (COSY, HSQC, HMBC, and INADEQUATE) spectra were acquired.
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We describe our results based on the 1H NMR spectral data with chemical shift changes, 2D 1H-1H COSY spectrum for assignment of protons and 1H-1H ROEspectrumrum together with molecular docking approaches thus elucidating the structure of the β-CD-FLN inclusion complex.
The assignment of protons that are involved in amide S H-bonds is more difficult due to their broad features that overlap with other protons.
Complete assignments of proton and carbon signals were performed by 2D NMR experiments.
Open image in new window Fig. 3 Liquid state 1H NMR spectrum of a ASDP and b ASWL asphaltenes Table 5 Assignments of proton chemical shift NMR spectra and average molecular parameters of (AS DP and (AS WL asphaltenes molecules calculated from the correlation Eqs.
The assignments of proton and proton-bearing carbon signals in the NMR spectra were confirmed by cross-peaks in the H-H COSY and HSQC spectra.
Assignments of proton, carbon, and phosphorous resonances of the species were obtained by one- and two-dimensional NMR spectra (H, P, H,C-HSQC, H,C-HMBC, H,H-ROESY and H,H-NOESY (mixing times of 600, 350 and 100 ms) spectra.
The assignments of protons for Hα-1/Hβ-1, Hα-10/Hβ-10, and H3-12/H3-13 were also established on the basis of the NOESY correlations.
Sequence-specific resonance assignments of protons have been made with the aid of correlation spectroscopy experiments and nuclear Overhauser effect spectroscopy experiments.
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