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Title: X-ray Crystallographic, Scanning Microprobe X-ray Diffraction, and Cross-Polarized/Magic Angle Spinning [superscript 13]C NMR Studies of the Structure of Cellulose III[subscript II]

Abstract

The X-ray crystallographic structure of cellulose III{sub II} is characterized by disorder; the unit cell (space group P2{sub 1}; a = 4.45 {angstrom}, b = 7.64 {angstrom}, c = 10.36 {angstrom}, {alpha} = {beta} = 90{sup o}, {gamma} = 106.96{sup o}) is occupied by one chain that is the average of statistically disordered antiparallel chains. {sup 13}C CP/MAS NMR studies reveal the presence of three distinct molecular conformations that can be interpreted as a mixture of two different crystal forms, one equivalent to cellulose III{sub I}, and another with two independent glucosyl conformations in the asymmetric unit. Both X-ray crystallographic and {sup 13}C NMR spectroscopic results are consistent with an aggregated microdomain structure for cellulose III{sub II}. This structure can be generated from a new crystal form (space group P2{sub 1}; a = 4.45 {angstrom}, b = 14.64 {angstrom}, c = 10.36 {angstrom}, {alpha} = {beta} = 90{sup o}, {gamma} = 90.05{sup o}; two crystallographically independent and antiparallel chains; gt hydroxymethyl groups) by multiple dislocation defects. These defects produce microdomains of the new crystal form and cellulose III{sub I} that scanning microprobe diffraction studies show are distributed consistently through the cellulose III{sub II} fiber.

Authors:
; ; ;
Publication Date:
Research Org.:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1005472
Resource Type:
Journal Article
Journal Name:
Biomacromolecules
Additional Journal Information:
Journal Volume: 10; Journal Issue: (2) ; 2009
Country of Publication:
United States
Language:
ENGLISH
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CELLULOSE; DISLOCATIONS; X-RAY DIFFRACTION; CRYSTAL STRUCTURE; NUCLEAR MAGNETIC RESONANCE; CARBON 13

Citation Formats

Wada, Masahisa, Heux, Laurent, Nishiyama, Yoshiharu, Langan, Paul, U of Tokyo), CNRS-CRMD), and LANL). X-ray Crystallographic, Scanning Microprobe X-ray Diffraction, and Cross-Polarized/Magic Angle Spinning [superscript 13]C NMR Studies of the Structure of Cellulose III[subscript II]. United States: N. p., 2009. Web. doi:10.1021/bm8010227.
Wada, Masahisa, Heux, Laurent, Nishiyama, Yoshiharu, Langan, Paul, U of Tokyo), CNRS-CRMD), & LANL). X-ray Crystallographic, Scanning Microprobe X-ray Diffraction, and Cross-Polarized/Magic Angle Spinning [superscript 13]C NMR Studies of the Structure of Cellulose III[subscript II]. United States. https://doi.org/10.1021/bm8010227
Wada, Masahisa, Heux, Laurent, Nishiyama, Yoshiharu, Langan, Paul, U of Tokyo), CNRS-CRMD), and LANL). 2009. "X-ray Crystallographic, Scanning Microprobe X-ray Diffraction, and Cross-Polarized/Magic Angle Spinning [superscript 13]C NMR Studies of the Structure of Cellulose III[subscript II]". United States. https://doi.org/10.1021/bm8010227.
@article{osti_1005472,
title = {X-ray Crystallographic, Scanning Microprobe X-ray Diffraction, and Cross-Polarized/Magic Angle Spinning [superscript 13]C NMR Studies of the Structure of Cellulose III[subscript II]},
author = {Wada, Masahisa and Heux, Laurent and Nishiyama, Yoshiharu and Langan, Paul and U of Tokyo) and CNRS-CRMD) and LANL)},
abstractNote = {The X-ray crystallographic structure of cellulose III{sub II} is characterized by disorder; the unit cell (space group P2{sub 1}; a = 4.45 {angstrom}, b = 7.64 {angstrom}, c = 10.36 {angstrom}, {alpha} = {beta} = 90{sup o}, {gamma} = 106.96{sup o}) is occupied by one chain that is the average of statistically disordered antiparallel chains. {sup 13}C CP/MAS NMR studies reveal the presence of three distinct molecular conformations that can be interpreted as a mixture of two different crystal forms, one equivalent to cellulose III{sub I}, and another with two independent glucosyl conformations in the asymmetric unit. Both X-ray crystallographic and {sup 13}C NMR spectroscopic results are consistent with an aggregated microdomain structure for cellulose III{sub II}. This structure can be generated from a new crystal form (space group P2{sub 1}; a = 4.45 {angstrom}, b = 14.64 {angstrom}, c = 10.36 {angstrom}, {alpha} = {beta} = 90{sup o}, {gamma} = 90.05{sup o}; two crystallographically independent and antiparallel chains; gt hydroxymethyl groups) by multiple dislocation defects. These defects produce microdomains of the new crystal form and cellulose III{sub I} that scanning microprobe diffraction studies show are distributed consistently through the cellulose III{sub II} fiber.},
doi = {10.1021/bm8010227},
url = {https://www.osti.gov/biblio/1005472}, journal = {Biomacromolecules},
number = (2) ; 2009,
volume = 10,
place = {United States},
year = {Mon Mar 16 00:00:00 EDT 2009},
month = {Mon Mar 16 00:00:00 EDT 2009}
}