Characterization of the ionic clathrate hydrate of tetra-<i>n</i>-butylammonium acrylate

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  • Sanehiro Muromachi
    National Institute of Advanced Industrial Science and Technology (AIST), 16-1 Onogawa, Tsukuba 305-8569, Japan.
  • Masato Kida
    National Institute of Advanced Industrial Science and Technology (AIST), 16-1 Onogawa, Tsukuba 305-8569, Japan.
  • Satoshi Takeya
    National Institute of Advanced Industrial Science and Technology (AIST), 16-1 Onogawa, Tsukuba 305-8569, Japan.
  • Yoshitaka Yamamoto
    National Institute of Advanced Industrial Science and Technology (AIST), 16-1 Onogawa, Tsukuba 305-8569, Japan.
  • Ryo Ohmura
    Department of Mechanical Engineering, Keio University, Yokohama 223-8522, Japan.

抄録

<jats:p> The ionic clathrate hydrate of tetra-n-butylammonium (TBA) acrylate was characterized using single-crystal X-ray diffraction, elemental analysis, and nuclear magnetic resonance (NMR) spectroscopy. The crystal structure of TBA acrylate was Jeffrey’s type III and tetragonal P4<jats:sub>2</jats:sub>/n, with a 33.076(7) × 33.076(7) × 12.170(2) Å<jats:sup>3</jats:sup> unit cell. The volume of the unit cell was 13315(5) Å<jats:sup>3</jats:sup>, which is almost twice that of the ideal structure. The TBA cation was disordered and located in two types of fused cages. Although the acrylate anion was located in a pentagonal dodecahedral cage neighboring the TBA cation, there is a residual acrylate anion that could be around the other TBA cation in the unit cell. Solid-state <jats:sup>13</jats:sup>C NMR spectra showed that the TBA cation was clearly disordered at 173 K, but not at 239 K. NMR peaks from the acrylate anion were not observed at either temperature. This is probably because of the strong restriction on the acrylate anion by hydrogen bonding with the lattice water. Some of the characteristics of the anion and cation of the ionic guest incorporated in the hydrate structure have yet to be defined. Further research is needed to clarify complexation of the ionic clathrate hydrate and the ionic guest, and the resulting structure. </jats:p>

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