TABLE 1.

NMR chemical shift assignments for 1,20,23(OH)₃D₃ and vitamin D₃ from analysis of their NMR spectra, and carbon chemical shifts obtained from detected signals in HSQC and heteronuclear multiple bond correlation experiments

Solvent was CD₃OD.

Atom	1,20,23(OH)3D3		D3
	1H	13C	1H	13C
1	4.36 β (t, J = 5.7Hz)	70.1	2.12 α, 2.40 β	33.8
2	1.89 α, 1.89 β	42.3	1.98 α, 1.54 β	36.8
3	4.13	66.1	3.76	70.7
4	2.52 α, 2.27 β	44.9	2.53 α, 2.19 β	47.2
5	N.A.	134.5	N.A.	137.5
6	6.33	123.7	6.22	122.8
7	6.09	118.1	6.04	119.1
8	N.A.	—a	N.A.	142.7
9	1.68 α, 2.87 β	28.7	1.69 α, 2.86 β	30.1
10	N.A.	148.6	N.A.	147.1
11	—	—	1.55 α, 1.67 β	24.7
12	1.39 α, 2.13 β	41.1	1.33 α, 2.03 β	42.1
13	N.A.	45.9	N.A.	47.1
14	2.01	56.5	2.02	57.7
15	1.52 α, 1.52 β	21.7	1.46 α, 1.46 β	23.4
16	1.75 α, 1.83 β	21.8	1.31 α, 1.91 β	28.9
17	1.65	60.8	1.30	58.1
18	0.71	12.9	0.56	12.5
19	4.91, 5.30	110.8	4.75, 5.04	112.8
20	N.A.	75.9	1.40	37.6
21	1.37	25.3	0.95	19.6
22	1.64, 1.46	47.1	1.39, 1.04	37.5
23	4.04	66.8	1.39, 1.19	25.1
24	1.16, 1.39	47.6	1.16	40.8
25	1.73	24.1	1.54	29.3
26,27	0.92	21.5	0.89	23.2

N.A., not applicable (ternary carbons).

^a —, chemical shifts could not be unambiguously determined because of overlapping or weak signals at this position.