The structure of the complex of cellulose I with ethylenediamine by X-ray crystallography and cross-polarization/magic angle spinning 13C nuclear magnetic resonance

Authors: Wada, Masahisa1; Heux, Laurent2; Nishiyama, Yoshiharu2; Langan, Paul3

Source: Cellulose, Volume 16, Number 6, December 2009 , pp. 943-957(15)

Publisher: Springer

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Abstract:

X-ray crystallographic and cross-polarization/magic angle spinning 13C nuclear magnetic resonance techniques have been used to study an ethylenediamine (EDA)-cellulose I complex, a transient structure in the cellulose I to cellulose IIII conversion. The crystal structure (space group P2 1 ; a = 4.546 Å, b = 11.330 Å, c = 10.368 Å and  = 94.017°) corresponds to a one-chain unit cell with one glucosyl residue in the asymmetric unit, a gt conformation for the hydroxymethyl group, and one EDA molecule per glucosyl residue. Unusually, there are no O–H···O hydrogen bonds between the cellulose chains; the chains are arranged in hydrophobic stacks, stabilized by hydrogen bonds to the amine groups of bridging EDA molecules. This new structure is an example of a complex in which the cellulose chains are isolated from each other, and provides a number of insights into the structural pathway followed during the conversion of cellulose I to cellulose IIII through EDA treatment.

Keywords: Cellulose; Ethylenediamine; NMR; X-ray crystallography

Document Type: Research Article

DOI: http://dx.doi.org/10.1007/s10570-009-9338-5

Affiliations: 1: Department of Biomaterials Science, Graduate School of Agricultural and Life Sciences, The University of Tokyo, Tokyo, 113-8657, Japan 2: Centre de Recherches sur les Macromolécules Végétales – CNRS, Affiliated with the Joseph Fourier University of Grenoble, BP 53, 38041, Grenoble Cedex 9, France 3: Bioscience Division, Los Alamos National Laboratory, Los Alamos, NM, 87545, USA, Email: langan_paul@lanl.gov

Publication date: December 1, 2009

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