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2D ROESY NMR combined with molecular modeling is an appropriate way to characterize the geometry of inclusion complexes.
2D NMR ROESY spectra for LAP-[beta]-CD inclusion complex were recorded at p[D.sup.*] 2, where LAP exhibits an appropriate solubility.
The relative configuration of 2 was the same as that of 1 by analysis of the [sup.1]H-[sup.1]H coupling constants and ROESY data (Figure S12) of 2.
The relative configurations for C-5, C-6, and C-7 in 3 were deduced to be the same as those in 1 by comparison of the coupling constants and ROESY data (Figure S18).
The assignments of the peptide resonances were made by a combination of mono- and bidimensional and multinuclear NMR techniques [sup.1]H-[sup.1]H TOCSY, [sup.1]H-[sup.13]C HSQC, and [sup.1]H-[sup.1]H ROESY at different pH values.
Structure calculations for the peptide-nickel complex were performed on the basis of the experimental evidences plus ROE cross-correlations observed in 2D [sup.1]H-[sup.1]H ROESY spectra.
On the basis of nuclear Overhauser effects observed via a two-dimensional ROESY experiment, we tentatively assign H2, H4b, H6, and H8b to pseudo-axial positions above the plane of Fig.
Furthermore, the nuclear Overhauser effect (NOE) cross-peaks between H-6 ([delta] 6.79) and both the anomeric proton ([delta] 5.29) and the methoxy group (8 3.88) were observed in the ROESY spectrum of M5-1 (Fig.
The [sup.1]H NMR, [sup.1]H-[sup.1]H COSY, HSQC, HMBC, and ROESY spectra of these metabolites were obtained (Table 2 and Fig.
The structure of the isolated compound (of purity [congruent to] 97%) was elucidated by correlations found in 2D COSY, ROESY, HSQC and HMBC spectra, and confirmed to be bakuchiol (Fig.
D-Side; Woodstar; Future Kings Of Spain; Laura Isibor; Roesy; Simple Kid.
The hitherto undetermined configurations at C-20 and C-22 of pseudojujubogenin were elucidated by phase-sensitive ROESY, and [.sup.1]H and [.sup.13]C signals of the saponins were assigned by DEPT, [.sup.1]H-[.sup.1]H COSY, HSQC and HMBC techniques.
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