Statistical approach for solid-state NMR spectra of a cellulose derived from a series of variable parameters
Keiko Okushita†‡, Takanori Komatsu†‡, Eisuke Chikayama†‡, and Jun Kikuchi†♯‡§*
†RIKEN Plant Science Center, 1-7-22 Suehiro-cho, Tsurumi-ku, Yokohama 235-0045, Japan.
♯Biomass Engineering Program, RIKEN Research Cluster for Innovation
‡International Graduate School of Arts and Sciences, Yokohama City University, 1-7-29 Suehirocho, Tsurumi-ku, Yokohama 230-0045, Japan.
§Graduate School of Bioagricultural Sciences and School of Agricultural Sciences, Nagoya University, 1 Furo-cho, Chikusa-ku, Nagoya, 464-8601, Japan.
*To whom correspondence should be addressed. E-mail:
Supplementary Figure
Figure S1. Results of PCA performed using CPVC spectra (CT = 10 ms to 50 ms) of 13C BC. To extract the PC2 component of the first PCA (Figure 2) in more detail, this PCA was performed. In the score plot (a), components with a contact time of 10 ms to 50 ms were colored as light to dark. The contributions of PC1 and PC2 were 93.10 % and 4.99 %, respectively. In the loading plot (b), PC1 and PC2 were plotted as gray and black, respectively. The bold bars show the 5 % level of the rejection rate in t-distribution of the loading values.
Figure S2. (a) 3D structure of cellobiose unit in cellulose Ia, whose structure was down loaded from Protein Data Bank. (b) Proton distance matrix of the cellulose Ia structure. The first raw and column correspond to the label of proton in (a). Calculated distance (Å) between the raw proton and the column proton was inserted into a cell of the matrix. The cells with relatively short distance were colored with the gradation of green (0.16 nm) to yellow (0.26 nm). The scale of 0.26 nm is almost corresponding to the distance r which was calculated from the formula r2 = aDtsd, inserting the values of a = 4/3, D = 0.5 nm2/ms1, and tsd = 0.1 ms. The spin diffusion time tsd = 0.1 ms was chosen because the boundary contact time between the first PC1 and PC2 (Figure 2(a)) was 100 ms.
Figure S3. Results of PCA performed using the raw CPVC spectra (Figure 1(b)) of 13C BC. In the score plot (a), components with a contact time of 10 ms to 5000 ms were colored as light to dark. The contributions of PC1 and PC2 were 98.49 % and 1.43 %, respectively. In the loading plot (b), PC1 and PC2 were plotted as gray and black, respectively.
Figure S4. Comparison of spectra with CT of 20 ms, 100 ms, and 250 ms. (a)The raw intensity spectra. (b) and (c) the normalized spectra.
Supplementary Reference
1. Masuda, K.,Adachi, M.,Hirai, A.,Yamamoto, H.,Kaji, H.,Horii, F., Solid-state C-13 and H-1 spin diffusion NMR analyses of the microfibril structure for bacterial cellulose. Solid State Nuclear Magnetic Resonance, 23, 198-212 (2003).