2D1H-1H and1H-13C NMR spectra of the composing units of PpFucCS.A, the overlayed COSY (green), TOCSY (magenta), and 150 ms mixing time NOESY (gray) spectral strip from the anomeric region (δH/δH expansions 5.8–5.0/6.0–3.25 ppm) shows the presence of four spin systems (vertical dashed lines) corresponding to four α-fucose (Fuc) units labeled as A–D, respectively, Fuc2,4S, Fuc2,4S, Fuc 4S, and Fuc. U denotes signals corresponding to glucuronic acid. B, δH/δH expansions 4.8 to 4.5/6.0 to 3.25 ppm in TOCSY spectrum covering the anomeric region of N-acetylgalactosamine (GalNAc) units, showing the presence of three spin systems (vertical dashed lines) corresponding to the non-, 6-, and 4-sulfated GalNAc units labeled, respectively, as N0S, N6S, and N4S. Pairs of numbers between parentheses indicate position of the 1H nuclei assigned in the cross-peaks, marked by circles. C and D, 1H-13C HSQC spectrum (δH/δC expansions 6.0–3.25/112.0–45.0 ppm, and δH/δC expansions 2.5–1.0/30.0–10.0 ppm), showing all 1H-13C cross-peaks of PpFucCS. All 2D NMR spectra were acquired at 50 °C on a 600 MHz Bruker NMR instrument. Labels on 1H-13C cross-peaks of (C) and (D) follow the same patterns of (A) and (B).