Table 2.
The 1H and 13C NMR chemical shifts and selected inter-residue correlations from NOESY and HMBC spectra of [ECA]-core glycoform isolated from E. coli R1.
| Residue | Chemical Shifts (ppm) | Selected Inter-Residue NOE and 3JH,C Connectivities | |||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|
| H1 C1 |
H2,(H3′) C2 |
H3 C3 |
H4 C4 |
H5 C5 |
H6,H6′ C6 |
H7, H7′ C7 |
H8,H8′ C8 |
H1/C1 Connectivities to |
Inter-Residue Atom/Residue | ||
| A | →5)-α-Kdop | nd | (2.27) 96.2 |
1.91 34.2 |
4.13 66.4 |
4.18 73.4 |
3.70 69.9 |
3.81 73.0 |
3.47, 3.94 64.9 |
||
| B | →3)-l-α-d-Hepp4PPEtn-(1→ | 5.21 100.2 |
4.02 71.8 |
4.09 78.6 |
4.64 72.4 |
4.24 72.1 |
4.11 69.4 |
3.73 63.9 |
4.18 | H5 of A | |
| C | →3,7)-l-α-d-Hepp4P-(1→ | 5.11 103.7 |
4.40 70.6 |
4.12 79.9 |
4.42 69.5 |
3.81 73.3 |
4.23 68.8 |
3.61, 3.77 68.5 |
4.09 78.6 |
C3, H3 of B | |
| D | l-α-d-Hepp-(1→ | 5.00 100.3 |
3.94 70.9 |
3.89 71.5 |
3.86 67.0 |
3.63 72.0 |
4.05 69.6 |
3.64, 3.75 63.7 |
3.61, 3.77 a 68.5 |
C7, H7,7′ of C | |
| E | →3)-α-d-Glcp-(1→ | 5.21 102.1 |
3.68 71.2 |
4.09 76.8 |
3.80 71.3 |
3.92 73.2 |
3.81, 3.92 60.7 |
4.12 a | H3 of C | ||
| F | →2,3)-α-d-Glcp-(1→ | 5.81 95.4 |
3.88 73.5 |
4.18 78.7 |
3.58 68.8 |
4.11 72.1 |
3.79, 4.00 61.1 |
4.09 76.8 |
C3, H3 of E | ||
| G | →2)-α-d-Galp-(1→ | 5.63 92.1 |
4.00 73.2 |
4.20 68.9 |
3.99 70.9 |
4.15 72.2 |
3.76 62.1 |
3.88 a | H2 of F | ||
| H | α-d-Galp-(1→ | 5.32 96.6 |
3.86 69.2 |
3.96 70.2 |
4.00 70.2 |
4.14 72.1 |
3.75 62.1 |
4.00 | H2 of G | ||
| I | →3)-β-d-Glcp-(1→ | 4.74 103.2 |
3.39 73.7 |
3.70 85.5 |
3.50 69.0 |
3.45 76.3 |
3.75, 3.91 61.5 |
4.18 78.7 |
C3, H3 of F | ||
| I’ b | β-d-Glcp-(1→ | 4.76 103.2 |
3.34 74.0 |
3.53 76.7 |
3.43 70.5 |
3.45 76.6 |
3.92, 3.74 61.5 |
4.18 78.7 |
C3, H3 of F | ||
| J | →4)-β-d-GlcpNAc-(1→ | 4.79 102.4 |
3.76 56.4 |
3.75 72.8 |
3.70 79.6 |
3.55 75.2 |
3.73, 3.86 61.0 |
3.70 85.5 |
C3, H3 of I | ||
| K | →4)-β-d-ManpNAcA-(1→ | 4.94 99.8 |
4.51 54.3 |
4.08 73.3 |
3.84 74.9 |
3.88 77.2 |
- 175.1 |
3.70 a 79.6 |
C4, H4 of J | ||
| L | α-d-Fucp4NAc-(1→ | 5.36 99.7 |
3.65 69.3 |
3.97 69.2 |
4.21 54.7 |
4.19 66.7 |
1.06 16.3 |
3.84 | H4 of K | ||
| PPEtn | 4.21 63.2 |
3.30 40.8 |
|||||||||
Anomeric configuration was determined on the basis of 3JH1,C1 coupling constant for following residues: B—174 Hz; C—171 Hz; D—172 Hz; E—173 Hz; F—175 Hz; G—172 Hz; H—173 Hz; I—163 Hz; J—162 Hz; K—163 Hz; L—175 Hz. a The value represents NOE connectivity only; b Residue I’ is a terminal residue I present in the core OS that was devoid of ECA trisaccharide; nd—not determined.