  The molecular structure and dynamics of regioregulated poly(3-butylthiophene)
(P3BT), poly(3-hexylthiophene)(P3HT), and poly(3-dodecylthiophene) (P3DDT) were
investigated using Fourier transform infrared absorption (FTIR), solid state
$^{13}$C nuclear magnetic resonance (NMR), and differential scanning
calorimetry (DSC) measurements. In the DSC measurements, the endothermic peak
was obtained around 340 K in P3BT, and assigned to enthalpy relaxation that
originated from the glass transition of the thiophene ring twist in crystalline
phase from results of FTIR, $^{13}$C cross-polarization and magic-angle
spinning (CPMAS) NMR, $^{13}$C spin-lattice relaxation time measurements, and
centerband-only detection of exchange (CODEX) measurements. We defined this
transition as {\it twist-glass transition}, which is analogous to the plastic
crystal - glassy crystal transition.
