논문 상세보기
pp.204-211
The structure of nitrogen adsorption complex of fully dehydrated Cd2+ ion exchanged zeolite-X, |Cd46(N)18|[Si100Al92O384], was determined in the cubic space group Fd3 at 21(1) ℃ [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(NO3)2 : Cd(O2CCH3)2 = 1:1 for five days, followed by dehydration at 500℃ and 2×10-6 Tor. for two days, and exposured to 100 Tor. zeolitically dry nitrogen gas at 21(1) ℃. The structure was determined in atmosphere, and was refined within F0 〉 4Σ(F0) using reflection for which the final error can appear in indices R1 = 0.097 and wR2 = 0.150. In this structure, Cd2+ ions occupied four crystallographic sites. Nine Cd2+ ions filled the octahedral site I at the centers of hexagonal prisms (Cd-O = 2.452(16) a). Eight Cd2+ ions filled site I' (Cd-O = 2.324(19) a). The remaining 29 Cd2+ ions are found at two nonequivalent sites II (in the supercages) with occupancy of 11 and 18 ions. Each of these Cd2+ ions coordinated to three framework oxygens, either at 2.159(15) or 2.147(14) a, respectively. Eighteen nitrogen molecules were adsorbed per unit cell and three per supercage.
