Through-bond assignment of sugar ¹H and ¹³C resonances

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Proton	Range 1H chemical shift	Range 13C chemical shift
1'	5.4-6.4	82.0-87.0
2'	2.0-3.0	38.0-41.0
2''	-	-
3'	4.5-5.2	70.0-79.0
4'	4.0-4.5	83.0-88.0
5'	3.6-4.4	61.0-68.0
5''	3.6-4.4	61.0-68.0

• Assignment of non-exchangeable sugar protons via NOE from 2D NOESY experiment and via J-coupling from 2D COSY and 2D TOCSY experiments. Overlapping can be resolved using hybrid experiments like 3D TOCSY-NOESY and 3D NOESY-NOESY
• Directly-attached ¹H-¹³C pairs are assigned from standard 2D ¹H-¹³C HMQC/ HSQC experiments.

• Stereospecific H5' and H5" proton assignments can be achieved from long-range proton-carbon coupling constants analysis extracted from multi-dimensional HMQC-TOCSY ( 93JACS11002 and 94JACS5823 ) or HMQC-NOESY ( 94JACS5823 ) experiments.Analysis of cross-peak signal intensities of C3'-H5 in 2D HMBC spectra can also be helpful
• Stereospecific H2' and H2" proton assignments in deoxyribose can be achieved from intraresidue d_i(1':2',2") NOE cross-peak analysis or from the measurement of ³J_1'2' and ³J_1'2" coupling constants.