Table 3.
unit/ring | no. | 5
|
6
|
unit/ring | no. | 5
|
6
|
||||
---|---|---|---|---|---|---|---|---|---|---|---|
δC, mult | δH (J, Hz) | δC, mult | δH (J, Hz) | δC, mult | δH (J, Hz) | δC, mult | δH (J, Hz) | ||||
unit I | unit III | ||||||||||
C | 2 | 99.98, C | 100.00, C | I | 2 | 84.53, CH | 4.6620, ddd (8.2, 0.1,–0.5) | 100.38, C | |||
3 | 68.59, CH | 4.0246, d (3.1) | 68.48, CH | 3.9870, d (3.0) | 3 | 68.46, CH | 4.0860, ddd (8.7, 8.2, 5.7) | 67.73, CH | 4.0867, d (3.4) | ||
4 | 29.82, CH | 4.6816, d (3.1) | 29.78, CH | 4.6718, d (3.0) | 4 | 29.58, CH2 | 3.0091, dd (−16.5, 5.7) 2.5730, ddd (−16.5, 8.7,0.5) |
29.63, CH | 4.3001, d (3.4) | ||
A | 5 | 157.84, C | 157.90, C | G | 5 | 156.13, C | 150.70, C | ||||
6 | 97.74, CH | 6.0059, d (2.4) | 97.74, CH | 6.0327, d (2.3) | 6 | 96.28, CH | 6.0862, s | 110.18, C | |||
7 | 158.11, C | 158.15, C | 7 | 152.70, C | 152.96, C | ||||||
8 | 96.33, CH | 6.0483, d (2.4) | 96.34, CH | 6.0610, d (2.3) | 8 | 107.33, C | 97.27, CH | 6.2523, s | |||
9 | 154.33, C | 154.35, C | 9 | 151.12, C | 152.73, C | ||||||
10 | 103.67, C | 103.55, C | 10 | 103.28, C | 106.36, C | ||||||
B | 1′ | 132.67, C | 132.62, C | H | 1′ | 130.79, C | 132.09, C | ||||
2′ | 115.42, CH | 7.0972, dd (2.2, 0.2) | 115.21, CH | 7.0325, dd (2.2, 0.2) | 2′ | 116.03, CH | 6.9638, ddd (2.1, −0.5, <0.1c) | *115.59, CH | 7.1191, dd (2.2, < 0.1c) | ||
3′ | 145.61, C | 145.56, C | 3′ | 146.76, C | 145.72, C | ||||||
4′ | 146.27, C | 146.65, C | 4′ | 146.70, C | 146.92, C | ||||||
5′ | 115.64, CH | 6.7815, dd (8.3, 0.2) | *115.61, CH | 6.7469, dd (8.4, 0.2) | 5′ | 116.26, CH | 6.8303, dd (8.2, < 0.1c) | *115.60, CH | 6.8077, dd (8.3, <0.1c) | ||
6′ | 119.65, CH | 6.9929, dd (8.3, 2.2) | 119.76, CH | 6.9858, dd (8.4, 2.2) | 6′ | 120.73, CH | 6.8829, dd (8.2, 2.1) | 119.83, CH | 7.0109, dd (8.3, 2.2) | ||
unit II | unit IV | ||||||||||
F | 2 | 100.76, C | 100.95, C | L | 2 | 85.00, CH | 4.6119, ddd (9.1, −0.2, 0.1) | ||||
3 | 67.82, CH | 4.0997, d (3.2) | 67.57, CH | 4.1187, d (3.1) | 3 | 68.01, CH | 4.2543, ddd (9.1,9.1,6.1) | ||||
4 | 29.65, CH | 4.3194, d (3.2) | 30.15, CH | 4.3878, d (3.1) | 4 | 30.61, CH2 | 3.1288 dd (−16.4, 6.1) 2.5768, ddd (−16.4, 9.1,0.1) |
||||
D | 5 | 155.85, C | 155.51, C | J | 5 | 156.31, C | |||||
6 | 98.12, CH | 6.1168, s | 98.11, CH | 6.1955, s | 6 | 96.61, CH | 6.0824, s | ||||
7 | 153.45, C | 153.56, C | 7 | 152.26, C | |||||||
8 | 108.80, C | 109.12, C | 8 | 106.38, C | |||||||
9 | 148.97, C | 148.89, C | 9 | 151.69, C | |||||||
10 | 105.42, C | 105.19, C | 10 | 103.71, C | |||||||
E | 1′ | 132.41, C | 132.31, C | K | 1′ | 130.22, C | |||||
2′ | 115.50, CH | 7.4033, dd (2.2, 0.2) | 115.53, CH | 7.4221, dd (2.2, < 0.1c) | 2′ | 117.27, CH | 7.0656, ddd (2.0, −0.2, 0.2) | ||||
3′ | 145.61, C | 145.62, C | 3′ | 146.23, C | |||||||
4′ | 146.89, C | 146.86, C | 4′ | 147.06, C | |||||||
5′ | 115.68, CH | 6.8809, dd (8.3, 0.2) | 115.70, CH | 6.8914, dd (8.3, < 0.1c) | 5′ | 116.69, CH | 6.9201, dd (8.2, 0.2) | ||||
6′ | 120.30, CH | 7.4232, dd (8.3, 2.2) | 120.34, CH | 7.4374, dd (8.3, 2.2) | 6′ | 121.04, CH | 7.0707, dd (8.2, 2.0) |
1H and 13C NMR data were acquired in methanol-d6 at 298 K at 900 and 225 MHz, respectively.
The δH and J values including their signs were generated via 1H iterative full spin analysis (HiFSA).11
Very small couplings were detected by HiFSA (for pms profiles, see the Supporting Information) and are essential for the line overall fit. Asterisks indicate that the signals are interchangeable.