Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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The Crystal Structure of Dehydrated Fully $Ag^+$-Exchanged Zeolite A Successively Treated with Ethylene and Bromine Vapor

  • Jeong, Mi-Suk (Department of Chemistry, Pusan National University) ;
  • Jang, Se-Bok (Department of Chemistry, Pusan National University) ;
  • Kim, Yang (Department of Chemistry, Pusan National University)
  • Published : 1994.11.20
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Abstract

The crystal structure of an ethylene sorption complex of dehydrated $Ag_{12}-A $reacted with bromine vapor has determined by single-crystal X-ray diffraction techniques in the cubic space group of Pm3m at 22(l)$^{\circ}$C (a=12.180(2) ${\AA}$). The crystal was prepared by dehydration of $Ag_{12}$-A at 400 $^{\circ}$C and $2 {\times} l0^{-6}$ Torr for 2 days, followed by exposure to 200 Torr of ethylene gas at 24(l) $^{\circ}$C for 1 hr. After the ethylene gas was evacuated for 1 hr, the crystal was exposed to 180 Torr of bromine vapor at 24(l) $^{\circ}$C for 1.5 h. The structure was refined to the final error indices, $R_1=0.066\;and\;R_2$ (weighted)=0.055, using 137 independent reflections for which I>3${\sigma}$I. About 55% of the sodalite unit contain two 6-ring $Ag^+$ ions and the remaining 45% contain $Ag_6$ molecules complexed to 2 $Ag^+$ ions at 6-ring sites to give $(Ag^+)_2(Ag_6).$ Upon sorption of ethylene, 4.75 ethylene molecules were sorbed per unit cell and of these, only 1.25 ethylene molecules were brominated by treatment of dibromine because of the limitation of the available space for the reaction products in the large cavity. In the large cavity, each of 3.5 $Ag^+$ ions forms a lateral ${\pi}$ complex with an ethylene molecule. About 2.5 8-ring $Ag^+$ ions per unit cell interact with 1.25 1,2-dibromoethane and each of ca. 1.25 6-ring $Ag^+$ ions also interacts with one of bromine atoms of 1,2-dibromoethane. Each bromine atom approaches a carbon atom with C-Br(l)=2.07(20) ${\AA}$ and C-Br(2)=2.07(10) ${\AA}$, respectively.

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References

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  1. Framework-Type Determination for Zeolite Structures in the Inorganic Crystal Structure Database vol.39, pp.3, 1994, https://doi.org/10.1063/1.3432459