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Crystal Structure and Morphology of Poly(16-hexadecalactone) Chain-folded Lamellar Crystals
Kim, Eunju,Uyama, Hiroshi,Doi, Yoshiharu,Ha, Chang-Sik,Iwata, Tadahisa WILEY-VCH Verlag 2005 Macromolecular bioscience Vol.5 No.8
<P>Summary: Solution-grown, chain-folded lamellar crystals of poly(16-hexadecalactone) (PHDL) were crystallized isothermally from 1-hexanol at 70 °C. The morphology of lozenge-shaped crystals was studied by TEM and AFM. The lamellae are ca. 10 nm thick and the chains run orthogonal to the lamellar surface with folding along (110) and (<TEX>$1\bar 10$</TEX>) planes. The crystal structure of PHDL was determined by XRD and election diffraction of single crystals. The chains are in the 2<SUB>1</SUB> helix conformation close to all-trans and the structure consists of an orthorhombic unit cell with a P2<SUB>1</SUB>2<SUB>1</SUB>2<SUB>1</SUB> space group with the lattice constants a = 0.746 ± 0.001 nm, b = 0.504 ± 0.001 nm, and c (chain axis) = 4.116 ± 0.003 nm. There are two chains per unit cell, which exist in an antiparallel arrangement. Molecular packing structure has been studied in detail, taking into account both diffraction data and energy calculations. The setting angles, with respect to a axis, were ±40° for the corner and center chains, respectively. By using the electron and XRD data, the best molecular packing model was refined to R-factors of 0.168 and 0.196, respectively. A brief comparison of chain-packing structure is also made with related polymer structures.</P><P> <img src='wiley_img/16165187-2005-5-8-MABI200500038-gra001.gif' alt='wiley_img/16165187-2005-5-8-MABI200500038-gra001'> Graphic </P>