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Crystal Structure of Nitrogen Adsorption of $Cd^{2+}$ ion Exchanged Zeolite-X

카드늄으로 이온교환된 제올라이트 X의 질소 흡착 결정구조

  • Lee, Seok-Hee (Dept. of Science Education, Busan National University of Education) ;
  • Jeong, Gyoung-Hwa (Dept. of Chemistry, Pusan National University) ;
  • Kim, Nam-Seok (Dept. of Chemical Engineering, Changwon National University)
  • 이석희 (부산교육대학교 과학교육학과) ;
  • 정경화 (부산대학교 화학과) ;
  • 김남석 (창원대학교 화공시스템)
  • Published : 2005.09.30

Abstract

The structure of nitrogen adsorption complex of fully dehydrated $Cd^{2+}$ ion exchanged zeolite-X, $|Cd_{46}(N)_{18}|[Si_{100}Al_{92}O_{384}]$, was determined in the cubic space group $Fd\overline{3}$ at 21(1) $^{\circ}C$ [a = 24.863(4) ] by single crystal X-ray diffraction analysis. The crystal was prepared by ion exchange in a flowing steam of 0.05 M aqueous solution $Cd(NO_3)_2$ : $Cd(O_2CCH_3)_2$ = 1:1 for five days, followed by dehydration at $500^{\circ}C$ and $2{\times}10^{-6}$ Tor. for two days, and exposured to 100 Tor. zeolitically dry nitrogen gas at 21(1) $^{\circ}C$. The structure was determined in atmosphere, and was refined within $F_0$ > $4{\sigma}(F_0)$ using reflection for which the final error can appear in indices $R_1$ = 0.097 and $wR_2$ = 0.150. In this structure, $Cd^{2+}$ ions occupied four crystallographic sites. Nine $Cd^{2+}$ ions filled the octahedral site I at the centers of hexagonal prisms (Cd-O = 2.452(16) ${\AA}$). Eight $Cd^{2+}$ ions filled site I' (Cd-O = 2.324(19) ${\AA}$). The remaining 29 $Cd^{2+}$ ions are found at two nonequivalent sites II (in the supercages) with occupancy of 11 and 18 ions. Each of these $Cd^{2+}$ ions coordinated to three framework oxygens, either at 2.159(15) or 2.147(14) ${\AA}$, respectively. Eighteen nitrogen molecules were adsorbed per unit cell and three per supercage.

Keywords

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