The structures of partially dehydrated and partially Co 2? -exchanged zeolites X (Si/Al = 1.40) and Y (Si/ Al = 1.70) were determined by single-crystal synchrotron X-ray diffraction techniques in the cubic space group Fd 3m and were refined to the final error indices R 1 /wR 2 = 0.0773/0.2152 and 0.0683/0.2184, respectively. Their unitcell formulas are |Co 26.1 Na 21 (H 3 O) 7.1 (H 2 O) 14.2 |[Si 112 Al 80 O 384 ]-FAU (a = 24.7892(2) Å ) and |Co 29.3 Na 6.2 (H 3 O) 5.9 (H 2 O) 5.9 |[Si 121 Al 71 O 384 ]-FAU (a = 24.7346 (2) Å ), respectively. In the structure of Co 2? -X, Co 2? ions occupy sites I 0 , II 0 , II, and III 0 ; the Na ? ions are at sites I 0 and II. In the structure of Co 2? -Y, Co 2? ions occupy sites I 0 , II 0 , II, and III 0 ; the Na ? ions are at site I 0 . Because of the low pH of the Co 2? exchange solution, some H 3 O ? ions are observed in both structures. The number of Co 2? ions in zeolite was increased slightly as Si/Al ratio increased, and Na ? content and the unit cell constant of the framework were decreased.Keywords Cobalt Á Partially dehydration Á Zeolites X and Y (FAU) Á Ion exchange Á Structure zeolites X and Y (FAU) have been determined by crystallographic method [14-16, 23, 24]. Three structures of Co 2? -exchanged zeolite X (Si/Al = 1.09) were determined by X-ray diffraction techniques [23]. Co 2? exchange was performed using 0.05 M aqueous CoCl 2 Á6H 2 O in the pH range 6-7 at 296 K (crystal 1), 323 K (crystal 2), and 353 K (crystal 3). In all the cases, excess Co 2? exchange with the uptake of OHwas observed. After partial dehydration at 296 K and ca. 0.13 Pa, the numbers of Co 2? , Na ? , H 3 O ? , and OHions in the three structures Electronic supplementary material The online version of this article (