Two-dimensional NMR data of a water-soluble β-(1→3, 1→6)-glucan from Aureobasidium pullulans and schizophyllan from Schizophyllum commune.

This article contains two-dimensional (2D) NMR experimental data, obtained by the Bruker BioSpin 500 MHz NMR spectrometer (Germany) which can used for the determination of primary structures of schizophyllan from Schizophyllum commune (SPG) and a water-soluble β-(1→3, 1→6)-glucan from Aureobasidium pullulans. Data include analyzed the 2D NMR spectra of these β-glucans, which are related to the subject of an article in Carbohydrate Polymers, entitled "NMR spectroscopic structural characterization of a water-soluble β-(1→3, 1→6)-glucan from A. pullulans" (Kono et al., 2017) [1]. Data can help to assign the 1H and 13C chemical shifts of the structurally complex polysaccharides.

Specifications Table

Value of the data

The following data detail NMR characterization of a novel water-soluble β-(1→3, 1→6)-glucan and schizophyllan from Schizophyllum commune.

The NMR data can be helpful to estimate the branching patterns of other β-glucans.

NMR parameters for the data can be useful for structural characterization of complex polysaccharides.

Data

The presented data include 2D NMR spectra of schizophyllan from Schizophyllum commune (SPG) and a water-soluble β-(1→3, 1→6)-glucan from Aureobasidium pullulans (A. pullulans) whose primary structures are shown in Fig. 1. 1H–13C heteronuclear single quantum coherence (HSQC), 2D 1H–13C heteronuclear multiple-bond correlation (HMBC), and 2D 1H–1H rotating frame Overhauser effect spectroscopy (ROESY) spectra of SPG are shown in Fig. 2, Fig. 3, Fig. 4, and those of the water-soluble A. pullulans β-(1→3, 1→6)-glucan are in Fig. 5, Fig. 6, Fig. 7, respectively.

Fig. 1

Primary structures of schizophyllan (SPG) and the water-soluble β-(1→3, 1→6)-glucan from A. pullulans. The A1, B1, B2, and C1 residues in SPG and A1, A2, B1, B2, C1, and C2 residues in the β-(1→3, 1→6)-glucan are magnetically inequivalent in their structures.

Fig. 2

HSQC spectrum of SPG in DMSO-d at 363 K. The vicinal 1H–13C spin couplings of the A1, B1, B2, and C1 residues in SPG (Fig. 1) are denoted by solid red, solid and dashed blue, and solid green lines, respectively. 1H and 13C NMR spectra of SPG are shown in horizontal and vertical axes in the HSQC spectrum, respectively, and the 1H and 13C resonance assignments are indicated in the 1H and 13C spectra.

Fig. 3

HMBC spectrum of SPG in DMSO-d at 363 K. The arrows indicate the interresidual correlations between A1H1–B1C3, B1H1–B2C3, B2H1–A3C3, and C1H1–A1C6 via glycosidic bonds.

Fig. 4

ROESY spectrum of SPG in DMSO-d at 363 K. The arrows indicate the interresidual correlations between B1H3–A1H1, A1H3–B2H1, B2H3–B1H1, A1H6a–C1H1, and A1H6b–C1H1 via glycosidic bonds.

Fig. 5

HSQC spectrum of the water-soluble β-(1→3, 1→6)-glucan from A. pullulans in DMSO-d at 363 K. The vicinal 1H–13C spin couplings of the A1, A2, B1, B2, C1, and C2 residues in the β-(1→3, 1→6)-glucan (Fig. 1) are denoted by solid and dashed red, solid and dashed blue, and solid and dashed green lines, respectively. 1H and 13C NMR spectra of the β-(1→3, 1→6)-glucan are shown in horizontal and vertical axes in the HSQC spectrum, respectively, and the 1H and 13C resonance assignments are indicated in the 1H and 13C spectra.

Fig. 6

HMBC spectrum of the water-soluble β-(1→3, 1→6)-glucan from A. pullulans in DMSO-d at 363 K. The arrows indicate the inter-residual correlations between C1C1–A1H6a, C1C1–A1H6b, C2C1–A2H6a, C2C1–A2H6b, C1H1–A1C6, and C2H1–A2C6 via glycosidic bonds.

Fig. 7

ROESY spectrum of the water-soluble β-(1→3, 1→6)-glucan from A. pullulans in DMSO-d at 363 K. The arrows indicate the interresidual correlations between A2H3–B2H1, A1H3–A2H1, B1H3–A1H1, A2H3–B2H1, B2H3–B1H1, A2H6a–C2H1, A2H6b–C2H1, A1H6a–C1H1, and A1H6b–C1H1 via glycosidic bonds.

Experimental design, materials and methods

The experiment's planning, design, and data processing correspond to the protocol given in Refs. [1], [2].

Samples

SPG was purchased from InvivoGen (USA). The water-soluble A. pullulans β-(1→3, 1→6)-glucan was prepared according to a previously reported method [1], [2].

Description of the NMR experiments

Each sample was dissolved in 600 μL of DMSO-d6 (99.9% isotropic purity, Sigma-Aldrich (USA)). All NMR spectra were recorded on a Bruker AVIII 500 MHz spectrometer at 363 K. HSQC data were acquired on a 2048 × 256-point matrix for the full spectrum, with 96 scans per increment, and the interpulse delay which corresponded to 1/4 J was set to 3.44 ms. HMBC) data were acquired on a 1024 × 256-point matrix for the full spectrum, with 128 scans per increment, and the delay time for the evolution was set to 62.5 ms. ROESY data were acquired on a 2048 × 256-point matrix for the full spectrum with 64 scans per increment, and the mixing time was 200 ms. The repetition time of each 2D NMR experiment was 2 s, and all 2D NMR data were zero-filled to 2k in both dimensions prior to Fourier transformation. 1H and 13C chemical shifts were calibrated using the methyl resonances of DMSO at 2.52 ppm for 1H and 39.52 ppm for 13C.

Subject area	Chemistry
More specific subject area	Structural analysis
Type of data	NMR spectra
How data was acquired	NMR, Bruker BioSpin AVIII 500 MHz spectrometer
Data format	Analyzed
Experimental factors	About 30 mg of each sample dissolved in 600 μL of 99.9% dimethylsulfoxide (DMSO)-d6.
Experimental features	All NMR experiments were performed at 363 K.
Data source location	National Institute of Technology, Tomakomai College, Nishikioka 443, Tomakomai, Hokkaido 059 1275, Japan
Data accessibility	Data are with this article.