Table 2. NMR Data^a for Compound 2 in MeOD-d₄.

position	δC	δNb	δH (J in Hz)	gCOSY	gHMBC	NOE	13N-HMBC
ADDA
1	176.1
2	45.4		2.73 dq (10.7, 7.0)	3, 17	1, 3, 17	3, 17
3	56.2		4.57 dd (9.0, 10.7)	2, 4	2, 4, 5	2, 4, 5, 17
4	126.2		5.52 dd (9.0, 15.5)	3, 5	3, 6	3, 5, 17, 18
5	139.4		6.26 d (15.5)	4	3, 6, 7, 18	3, 4, 7, 17, 19
6	133.9
7	137.4		5.44 d (10.0)	8, 18	5, 8, 9, 18	5, 8, 9, 10a, 10b, 19
8	37.9		2.59 d pent (10.0, 6.7)	7, 9, 19	6, 7, 9, 10, 19	18, 19
9	88.5		3.26 m	8, 10a, 10b	7, 10, 11, 19, 20	Ar, 7, 19
10a	39.1		2.82 dd (5.0, 14.1)	9, 10b	8, 9, 11, 12, 16	12, 16, 19
10b			2.67 dd (7.3, 14.1)	9, 10a	8, 9, 11, 12, 16	12, 16
11	140.6
12	130.6		7.18 m		10, 14, 16	10a, 10b, 18, 19, 20
13	129.3		7.24 m		11, 15
14	127.1		7.17 m		12, 16
15	129.3		7.24 m		11, 13
16	130.6		7.18 m		10, 12, 14	10a, 10b, 18, 19, 20
17	16.4		1.05 d (7.0)	2	1, 2, 3	2, 17
18	13.0		1.60 d (1.1)	7	5, 6, 7	8, 12, 16, 19, 20
19	16.7		1.01 d (6.7)	8	7, 8, 9	8, 10a, 12, 16, 18
20	58.9		3.22 s		9	12, 16, 18
Val
21	171.3
22	58.1		4.43 d (4.1)	23, 22NH	21, 23, 24, 26	23, 24, 25	22-N
23	30.1		2.45 m	22, 24, 25		22, 24, 25	22-N
24	17.0		0.80 d (7.1)	23	22, 23, 25	22, 23
25	19.9		0.86 d (7.1)	23	22, 23, 24	22, 23
22-N		119.5	8.32 d (10.2)	22
βMeASP
26	176.8
27	39.8		3.19 dq (2.5, 7.0)	28, 30	26/29	28, 30	28-N
28	57.7		4.39 d (2.5)	27	27, 29, 30	27, 30
29	176.7
30	16.9		1.31 d (7.0)	27	26, 27, 28	27, 28
28-N		110.6	8.89 d (6.8)
NMeΔBUT
31	165.7
32	137.2
33	138.1		7.00 q (7.1)	34	31, 32, 34		32-N
34	13.4		1.77 d (7.1)	33	31, 32	35
35	35.2		3.11 s		32, 36	34	32-N
32-N		112.5
GLU
36	174.3
37a	29.5		2.45 m	37b, 38a, 38b
37b			2.05 m	37a, 38a
38a	27.8		2.17 m	38b, 39, 37a			39-N
38b			2.05 m	38a, 39
39	52.0		4.69 dd (3.9, 5.7)	38a, 38b		38a, 38b/37b
40	174.6
39-N		122.2

^aMeasured at 600 MHz (¹H) (also see Figure S4) and 125 MHz (¹³C).

^bNH₃ used as δ = 0 reference.