Crystalline structure of isotactic poly(vinylcyclobutane) from fiber diffraction spectra

The crystalline structure of isotactic poly(vinylcyclobutane), claimed to b e tetragonal, has been revised on the basis of fiber diffraction spectra. T he chain symmetry is 4(1), as already assessed, but the conformation is dif ferent (the identity period is 6.91 Angstrom and not 6.60 Angstrom). The sp ace group is the orthorhombic P2(1)2(1)2(1) with lattice constants a = 17.1 4 Angstrom, b = 8.99 Angstrom, and c = 6.91 Angstrom. The excellent quality of the oriented samples allowed a full structure analysis and refinement. Integrated diffraction intensities, from a stretched fiber, measured with a Fuji image plate detector, have been utilized in a constrained refinement (the helix was assumed strictly of 4(1) symmetry and the C-C bond lengths w ere set to 1.54 Angstrom) obtaining a final R index of 15%. The refined cha in bond angles are 103 and 107 degrees, and the chain torsion angles are 16 5 and 273 degrees.