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Structural study of a cyclopentane sorption complex of fully dehydrated H-ZSM-5 (Si/Al = 24), |H3.8(C5H10)1.47|[Al3.8Si92.2O192]-MFI

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Abstract

To study the cyclopentane sorption sites and the effect of sorption on the H-ZSM-5 structure, crystal of H-ZSM-5 were prepared by burning out the tetrapropylammonium cations in air. For the adsorption of cyclopentane into H-ZSM-5 crystal, the crystal was treated with zeolitically dried cyclopentane for 6 h at 297 K, and then evacuated for 600 s at this temperature and 1.1 × 10–4 Pa. The structure of a single crystal of cyclopentane sorption complex of dehydrated H-ZSM-5 (MFI, |H3.8(C5H10)1.47|[Al3.8Si92.2O192]-MFI, Si/Al = 24) has been determined crystallographically using synchrotron X-radiation in the orthorhombic space group Pnma; a = 20.141(4), b = 19.944(4), c = 13.439(3) Å. It was refined using all intensities to the final error indice R1 = 0.072. The 1.47 cyclopentane molecules per unit cell are located between 5-rings in zigzag channel. The cyclopentane molecules are located perpendicular to the 10-rings of zigzag channel and parallel to the 5-rings of H-ZSM-5 framework at the center of them. Each cyclopentane molecule is held in place by 16 hydrogen bonds between all hydrogen atoms of cyclopentane and framework oxygen atoms of its 5- and 10-rings: C···O ca. 3.318 ~ 3.992 Å.

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Acknowledgements

The authors wish to thank the staff of Photon Factory (Beamline BL-5A) of Japan, for their kind assistance during data collection. Following are results of a study on the “Leaders in Industry-university Cooperation +” Project, supported by the Ministry of Education and National Research Foundation of Korea.

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Author notes

  1. JongJin Kim and Sayantika Nath are the first two authors contributed equally to this work.

Authors and Affiliations

  1. Enbion Inc. 275, Techno 2-ro, Yuseong-gu, Daejeon, 34026, Korea

    Jong Jin Kim, Bong Been Yim & Hyun-Jae Lee

  2. Department of Applied Chemistry, Andong National University, Andong, 36729, Korea

    Sayantika Nath, Hu Sik Kim & Woo Taik Lim

  3. Department of Applied Chemistry, College of Engineering, Kyungpook National University, Daegu, 41566, Korea

    Nam Ho Heo

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  1. Jong Jin Kim
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Correspondence to Nam Ho Heo or Woo Taik Lim.

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Kim, J.J., Nath, S., Yim, B.B. et al. Structural study of a cyclopentane sorption complex of fully dehydrated H-ZSM-5 (Si/Al = 24), |H3.8(C5H10)1.47|[Al3.8Si92.2O192]-MFI. J Porous Mater 29, 73–86 (2022). https://doi.org/10.1007/s10934-021-01134-9

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