. Author manuscript; available in PMC: 2018 Sep 25.

Published in final edited form as: RSC Adv. 2017 Sep 25;7(72):45733–45751. doi: 10.1039/c7ra09602j

Table 1.

NMR spectroscopic data for compound 1 (700 and 175 MHz, ¹H and ¹³C, respectively) in DMSO-d₆

position	δ_C	type	δ_H, mult. (J in Hz)	position	δ_C	type	δ_H, mult. (J in Hz)

Ac				δ ₂			3.65^a
C═O	171.0	C		*Leu⁷*
CH₃	23.0	CH₃	1.91, s	C═O	172.6	C
*Aib¹*				α	53.1	CH	3.96^a
C═O	176.1	C		β ₁	38.7	CH₂	1.47^a
α	55.7	C		β ₂			1.85^a
β₁	23.8	CH₃	1.34, s	γ	24.4	CH	1.72^a
β₂	26.3	CH₃	1.36, s	δ₁	20.8	CH₃	0.83, d (6.6)
NH			8.77, s	δ₂	23.0	CH₃	0.92, d (6.6)
*Ser²*				NH			7.53, d (7.9)
C═O	171.2	C		*Leu⁸*
α	58.3	CH	3.99¹	C═O	172.2	C
β	60.5	CH₂	3.66–3.75, m	α	50.6	CH	4.29^a
NH			8.42, d (4.3)	β	39.6^a	CH₂	1.55^a
OH			5.34, brs	γ	24.1	CH	1.59^a
*Val³*				δ₁	20.3	CH₃	0.74, d (6.4)
C═O	171.5	C		δ₂	22.8	CH₃	0.79, d (6.4)
α	60.4	CH	3.86, dd (7.5, 7.4)	NH			7.16, d (9.1)
β	29.0	CH	2.13, dq-like (13.7, 6.9)	*Aib⁹*
γ₁	19.1	CH₃	0.89, d (6.8)	C═O	171.5	C
γ₁	18.9	CH₃	0.93, d (6.8)	α	55.7	C
NH			7.68, d (7.4)	β₁	25.5	CH₃	1.32, s
*Ile⁴*				β₂	23.8	CH₃	1.36, s
C═O	172.5	C		NH			7.52, s
α	57.6	CH	4.12, t (7.8)	*Pro¹⁰*
β	35.5	CH	1.89, m	C═O	171.1	C
γ_1a	24.6	CH₂	1.24, m	α	62.2	CH	4.24, dd (8.3, 6.4)
γ_1b			1.41, m	β₁	28.9	CH₂	1.64, m
δ	10.5	CH₃	0.76, t (7.4)	β₂			2.08, m
γ₂	15.5	CH₃	0.84, d (6.9)	γ	25.4	CH₂	1.76, m
NH			7.30, d (8.5)	δ₁	48.0	CH₂	3.22, dt (11.3, 7.2)
*Aib⁵*				δ₂			3.65, m
C═O	173.0	C		*Ileol¹¹*
α	56.1	C		α	54.5	CH	3.66^a
β₁	25.5	CH₃	1.38, s	β	34.9	CH	1.59^a
β₂	23.0	CH₃	1.45, s	γ_1a	23.9	CH₂	0.99, ddd (13.5, 9.2, 7.0)
NH			7.97, s	γ_1b			1.46^a
*Pro⁶*				δ	11.6	CH₃	0.83, t (7.5)
C═O	173.3	C		γ₂	16.0	CH₃	0.81, d (7.0)
α	63.3	CH	4.20, dd (8.1, 7.6)	β₁′	61.2	CH₂	3.36, dd (11.3, 6.7)
β₁	28.6	CH₂	1.59^a	β₂′			3.45^a
β₂			2.24, m	NH			7.02, d (9.4)
γ	25.7	CH₂	1.86^a	OH			3.98^a
δ₁	48.5	CH₂	3.39, dt (11.7, 7.9)

Overlapping signals; chemical shifts were determined from ¹H-¹³C HSQC correlations