Table 1.
1H and 13C-NMR chemical shifts and coupling constants of the sugar backbones of M. loti lipid A. Spectra were recorded at 600 MHz (1H) and 151 MHz (13C) in DMSO-d6/CDCl3 (1:1 [v/v]) at 323K
| Residue positions | β-GlcNNa (C) | α-GlcNN (B) | α-GalA (A) | |||
|---|---|---|---|---|---|---|
|
|
|
|
||||
| 1H | 13C | 1H | 13C | 1H | 13C | |
| Untreated lipid A | ||||||
| 1 | 4.46 (8.2) | 102.9 (161.6) | 4.86 (3.8) | 92.9 (177.1) | 4.98 (3.5) | 95.4 (176.3) |
| 2 | 3.63 | 54.9 | 3.84 | 52.4 | 3.76 | 68.6 |
| NH | 7.41 | 7.43 | ||||
| 3 | 4.00 | 54.3 | 4.10 | 52.1 | 3.92 | 69.3 |
| NH | 7.35 | 7.39 | ||||
| 4 | 4.06 | 72.0 | 3.29 | 69.3 | 4.08 | 71.2 |
| 5 | 3.26 | 77.6 | 3.97 | 72.5 | 4.39 | 71.6 |
| 6 | 3.64 | 62.2 | 3.60 | 69.1 | — | 171.2 |
| 3.71 | — | 3.85 | — | |||
| POMe | 3.44 (10.5) | 53.4 | ||||
| HF-treated lipid A | ||||||
| 1 | 4.38 (8.1) | 102.7 | 4.86 (3.2) | 93.0 | 4.98 (3.6) | 95.3 |
| 2 | 3.61 | 54.1 | 3.85 | 52.4 | 3.76 | 68.5 |
| NH | 7.41 | 7.43 | ||||
| 3 | 3.74 | 56.8 | 4.10 | 52.1 | 3.92 | (69.4) |
| NH | 7.48 | 7.40 | ||||
| 4 | 3.25 | 69.8 | 3.30 | 69.3 | 4.09 | 71.2 |
| 5 | 3.16 | 78.7 | 3.97 | 72.5 | 4.41 | 71.5 |
| 6 | 3.52 | 61.9 | 3.60 | 69.0 | — | NDb |
| 3.68 | — | 3.88 | — | |||
| HZ-treated lipid A | ||||||
| 1 | 4.42 (8.2) | 103.2 | 4.85 (3.4) | 92.9 | 4.98 (3.3) | 95.1 |
| 2 | 3.76 | 54.5 | 3.83 | 52.4 | 3.75 | 68.4 |
| NH | 7.41 | 7.44 | ||||
| 3 | 4.01 | 54.6 | 4.08 | 51.8 | 3.92 | (69.3) |
| NH | 7.35 | 7.39 | ||||
| 4 | 4.08 | 72.1 | 3.44 | 68.3 | 4.09 | 71.1 |
| 5 | 3.29 | 77.4 | 3.94 | 72.1 | 4.40 | 71.5 |
| 6 | 3.65 | 61.2 | 3.59 | 69.3 | — | 171.1 |
| 3.68 | — | 3.90 | — | |||
| POMe | 3.51 (10.9) | 53.9 | ||||
a
GlcNN: 2,3-diamino-2,3-dideoxyglucose (presumed)
b
ND: not determined