Ten signals were present in the anomeric region of the 1 HNMR (δH4.56.3; Figure S16, Supporting Information) and 13C NMR (δC95110; Figure S17, Supporting Information) spectra of 3, which allowed the number of sugar units in each pentasaccharide unit to be confirmed (Table 2). The nonanomeric signals of each monosaccharide unit were assigned by a combination of COSY (Figure S18, Supporting Information) and TOCSY (Figure S19, Supporting Information) experiments. In cases where it was not possible to assign specific methine resonances due to signal overlap, spectroscopic simulation by means of nonlinear fit of the 1H NMR spectrum throughan iterative process using the MestRe-C program was used to determine the correct assignment for the coupling constants of all superimposed protons in each monosaccharide unit