(FcCHCHPymCH3)x[Ni(dmit)2] complex was prepared by means of the electro-crystallization technique using a typical H-type cell.2 (FcCHCHPymCH3) [Ni(dmit)2]2 and [(n-C4H9)4N][Ni(dmit)2]11 were obtained according to the previously reported procedure. The IR spectra were obtained by the KBr pellet method on a MIDAC FT-IR spectrometer. The micro-Raman measurements were carried out at room temperature using a Raman microscope spectrometer (Renishaw Ltd.) equipped with an He:Ne (λo=6328Å) laser. The incident laser power applied was adjusted to as low as 0.06 mW, and was focused on a 1 μm2 area, because using a higher laser intensity caused the samples to burn. The samples were mounted on a glass microscope slide. Each spectrum was scanned over 20 times between 200 and 2000 cm-1 with a 200 sec time constant at a 1 cm-1 resolution, and the Raman shifts thereby obtained were calibrated against a standard Si peak at 520 cm-1. Typically, more than six hours was required for collecting the Raman data of each sample.