Abstract
Two crystal structures of fully dehydrated, fully Ag+-exchanged zeolite X have been determined by single-crystal X-ray diffraction techniques. Ion exchange was accomplished by allowing 0.05 M aqueous AgNO3 to flow past each crystal for 3 days to give hydrated Ag92Si100Al92O384. One crystal was dehydrated at 400 °C for 2 days, followed by cooling to 21 °C, all in a flowing stream of dry oxygen gas (790 Torr), followed by evacuation at 2 × 10-6 Torr for 20 min. The structure was determined in the cubic space group Fd3m (a = 25.177(4) A) and was refined to the final error indices R1 = 0.048 and R2 = 0.078 with 291 reflections for which I > 3σ(I). The second crystal (a = 24.871(4) A) was similarly dehydrated without oxygen. Its structure was determined in Fd3 and refined to R1 = 0.069 and R2 = 0.072 with 320 reflections as above. In the first crystal, 4 Ag+ ions were found at the octahedral site I (Ag+−O = 2.689(7) A) and 24 Ag+ ions occupy the nearby site I‘ positions (Ag+−O = 2.220(10) A), avoiding I−I‘ c...
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