Single-Crystal Structures of Li⁺-exchanged Zeolite X (FAU, Si/Al = 1.09) from Aqueous Solution Depends on Ion-exchange Temperatures at 293 and 333 K

Two single crystals of fully dehydrated partially $Li^+$-exchanged zeolite X were prepared by the exchange of Na-X, $Na_{92}Si_{100}Al_{92}O_{384}$ (Si/Al = 1.09), with $Li^+$ using aqueous 0.1 M $LiNO_3$ at 293 (crystal 1) and 333 K(crystal 2), followed by vacuum dehydration at 623 K and $1{\times}10^{-6}$ Torr for 2 days. Their structures were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group $Fd{\overline{3}}$ at 100(1) K. Their structures were refined using all intensities to the final error indices (using the 1281 and 883 reflections for which ($F_o$ > $4{\sigma}(F_o)$) $R_1/R_2$ = 0.075/0.244 and 0.074/0.223 for crystals 1 and 2, respectively. Their compositions are seen to be ${\mid}Li_{86}Na_6{\mid}[Si_{100}Al_{92}O_{384}]$-FAU and ${\mid}Li_{87}Na_5{\mid}[Si_{100}Al_{92}O_{384}]$-FAU, respectively. In crystal 1, 17 $Li^+$ ions per unit cell are at site I', 15 another site I', 30 at site II, and the remaining 16 at site III; 2 $Na^+$ ions are at site II and the remaining 4 at site III'. In crystal 2, 32 and 30 $Li^+$ ions per unit cell fill sites I' and II, respectively, and the remaining 25 at site III'; 2 and 3 $Na^+$ ions are found at sites II and III', respectively. The extent of $Li^+$ exchange increases slightly with increasing ion exchange temperature from 93% to 95%.