Li+-exchanged Zeolites X and Y (FAU) from Undried Formamide Solution

Two single-crystals of fully dehydrated, partially $Li^+$-exchanged zeolites X (Si/Al = 1.09, crystal 1) and Y (Si/Al = 1.56, crystal 2), were prepared by flow method using 0.1 M $LiNO_3$ at 393 K for 48 h, respectively, followed by vacuum dehydration at 673 K and $1{\times}10^{-6}$ Torr. Their structures were determined by single-crystal X-ray diffraction techniques in the cubic space group $Fd\bar{3}$ and $Fd\bar{3}m$ at 100(1) K for crystals 1 and 2, respectively. They were refined to the final error indices $R_1/wR_2$ = 0.065/0.211 and 0.043/0.169 for crystals 1 and 2, respectively. In crystal 1, about 53 $Li^+$ ions per unit cell are found at three distinct positions; 9 at site I', 19 at another site I', and the remaining 25 at site II. The residual 25 $Na^+$ ions occupy three equipoints; 2 are at site I, 7 at site II, and 16 at site III'. In crystal 2, about 31 $Li^+$ ions per unit cell occupy sites I' and II with occupancies at 22 and 9, respectively; 3, 4, 23, and 3 $Na^+$ ions are found at sites I, I', II, and III', respectively. The extent of $Li^+$ ion exchange into zeolite X (crystal 1) is higher than that of zeolite Y (crystal 2), ca. 73% and 56% in crystals 1 and 2, respectively.