A macroscopically oriented lamello-columnar mesophase was obtained from a newly designed and synthesized symmetric tetrathiafulvalene-based molecule (symTTF11) containing four flexible alkyl chains chemically attached to the periphery of TTF mesogens (L. Wang, et al., J. Mater. Chem., 2011, 21, 60), and its phase behaviors and physical properties were investigated by the combined experimental techniques. Based on the experimental results and structure analyses, it was revealed that there are two ordered columnar phases below the isotropic phase: a columnar crystalline phase (Col K ) and a columnar smectic liquid crystal phase (Col L ). From two-dimensional wide angle X-ray diffraction patterns of the macroscopically oriented samples, phase structures of Col K and Col L were identified and their biaxial molecular packing structures were also proposed. Since the assembled symTTF11 columns were well organized in the ordered layer structures over a macroscopic domain, symTTF11 exhibited a good charge carrier mobility in the Col L phase.

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