Table 1.
NMR data of 2-amino-5-oxocylohex-1-ene-1-carboxyl-CoA obtained in 19 mM phosphate buffer (pH 7.6) containing 10% D2O
| Position | Chemical shifts, ppm
|
Coupling constants, Hz
|
Isotope shifts¶, ppb
|
Correlation experiments
|
|||||
|---|---|---|---|---|---|---|---|---|---|
| 1H* | 13C† | JCC‡ | JCP§ | JHH§ | Δ1H(2H) | Δ13C(2H) | TOCSY | HMBC | |
| COSCoA | 190.42 | e1, 6 | |||||||
| 1 | 96.94 | 68.6(2), 46.9(6), 2.9 | 67(6) | 6, 3 | |||||
| 2 | 162.59 | 68.4(1), 40.6(3), 1.8 | 25(6) | 6, 3, 4 | |||||
| 3 | 2.55 (t) | 31.46 | 40.6(2), 31.6(4), 2.0 | 6.8 | 4 | 4 | |||
| 4 | 2.42 (t) | 38.61 | 39.6(5), 31.7(3), 10.0(6), 2.9 | 6.8 | 88(3) | 3 | 3.6(w) | ||
| 5 | 218.14 | 39.5(4), 37.8(6), 3.5 | 52(6) | 6, 3, 4 | |||||
| 6 | 3.01 (s) | 40.65 | 46.9(1), 37.7(5), 10.3(4), 1.8 | 22(6) | |||||
| a2 | 8.11 (s) | 155.38 | |||||||
| a4 | 151.85 | a8, a2, 1′(w) | |||||||
| a5 | 121.11 | a8, NH2-a10(w), a2(w) | |||||||
| a6 | 158.13 | a2 | |||||||
| a8 | 8.47(s) | 143.32 | 1′ | ||||||
| NH2-a10 | 6.85 (s) | ||||||||
| 1′ | 6.07 (d) | 89.21 | 7.4 | 2′, 3′, 4′ | 2′, 3′ | ||||
| 2′ | 4.76 (m) | 77.36 | 3.3 | ND | 3′, 4′, 1′ | 1′ | |||
| 3′ | 4.71 (m) | 76.49 | 5.3 | ND | 4′, 2′, 1′ | 4′, 5′ | |||
| 4′ | 4.52 (m) | 86.76 | ND | ND | 5′, 3′, 2′, 1′ | 3′, 5′, 1′(w) | |||
| 5′ | 4.18 (m) | 68.57 | 5.3 | ND | 4′ | 4′(w), 3′(w) | |||
| e1 | 2.84 (m) | 29.86 | ND | c2, NH-c3 | |||||
| e2 | 3.23 (m) | 42.29 | ND | e1, NH-e3 | NH-e3, e1(w) | ||||
| NH-e3 | 8.24 (t) | 5.7 | e2, e1 | ||||||
| p1 | 176.73 | NH-c3, p2, c2(w), p3(w) | |||||||
| p2 | 2.36 (t) | 38.21 | 6.5 | p3, NH-p4 | p3(w) | ||||
| p3 | 3.38 (m) | 38.35 | p2, NH-p4 | p2, NH-p4 | |||||
| NH-p4 | 8.10 (t) | 5.9 | p3, p2 | ||||||
| p5 | 177.69 | NH-p4, p6, p3(w) | |||||||
| p6 | 3.99 (s) | 76.70 | p8, p9, p10, p10′ | ||||||
| p7 | 41.09 | 8.2 | p8, p9, p6, p10(w), p10′(w) | ||||||
| p8 | 0.70 (s) | 20.76 | p6, p9, p10(w), p10′(w) | ||||||
| p9 | 0.85 (s) | 23.76 | p8, p6, p10, p10′ | ||||||
| p10 | 3.49 (dd) | 74.63 | 5.5 | 9.5, 4.7 | p10′ | p8, p9, p6 | |||
| p10′ | 3.80 (dd) | 9.5, 4.7 | p10 | p8, p9, p6 | |||||
ND, not determined; w, weak cross-peak intensity.
Referenced to external trimethylsilylpropanesulfonate; signal multiplicities are indicated in parentheses (s, singlet; d, doublet; t, triplet; m, multiplet; dd, double doublet).
Referenced to external trimethylsilylpropanesulfonate.
13C13C coupling constants as determined from 13C NMR signals of a sample obtained from [ring-13C6]AB-CoA; coupling partners as determined from INADEQUATE experiments are indicated in parentheses.
Obtained from one-dimensional spectra.
Obtained from one-dimensional 13C NMR data of deuterated isotopomers. The position of deuteration is specified in parentheses.