Solution NMR assignments
This protocol is extracted from research article:
Encoding canonical DNA quadruplex structure
Sci Adv, Aug 31, 2018; DOI: 10.1126/sciadv.aat3007

Proton assignments were performed following well-established procedures and, in some cases, aided by inosine substitutions. Identification of intranucleotide anomeric signals was derived from DQF-COSY (double quantum-filtered correlation spectroscopy) and TOCSY (total correlation spectroscopy) experiments. G-quadruplex sequence-specific assignments were based on sequential nuclear Overhauser effect (NOE) connectivities of the type H8/H6(i)-H1’(i)-H8/H6(i+1) and the corresponding sequential connectivities on H2′/H2″ and H3′ spin systems derived from nuclear Overhauser effect spectroscopy (NOESY) experiments. JR-NOESY experiments allowed for GH1 and GH21/GH22 assignments. Typically, (1H-31P)HSQC (heteronuclear single quantum correlation) experiments that allow for tracing intranucleotide spin system connectivities involving H3′(i-1)-P(i)-H4′/H5′/H5″(i) were acquired to support or identify residue sequential connectivities. In selected cases, unambiguous assignment of imino H1 from the aromatic H8 guanines in the stem was also performed from natural abundance JR [1H-13C] HMBC (heteronuclear multiple-bond correlation) experiments. The chemical shift assignments are shown in tables S1 to S7.

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