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The crystals of two isostructural uranyl selenates, M[(UO 2 )(SeO 4 ) 2 (H 2 O)](H 2 O) 4  (M = Mg, Zn), have been prepared by water evaporation from aqueous solutions. The structures have been solved by direct methods (M = Mg: P2 1 /c, a = 8.4666(8), b = 11.6306(14), c = 13.1669(12) Å , β = 90.959(7)°, V = 1296.4(2) Å 3 , R 1  = 0.061; M = Zn: P2 1 /c, a = 8.4492(18), b = 11.5860(17), c = 13.240(3) Å , β = 92.382(18)°, V = 1294.9(4) Å 3 , R 1  = 0.074). The structures are based upon [(UO 2 )(SeO 4 ) 2 (H 2 O)] 2−  chains running parallel to the b axis and consisting of corner-sharing [UO 6 (H 2 O)] 6−  pentagonal bipyramids and [SeO 4 ] 2−  tetrahedra. The equatorial planes of the uranyl pentagonal bipyramids are oriented approximately parallel to (001). The uranyl selenate chains are linked into sheets parallel to (010) by [M(H 2 O) 6 ] 2+  octahedra which share common H 2 O molecules with the [UO 6 (H 2 O)] 6−  pentagonal bipyramids.

Preparation and Crystal Structures of M[(UO 2 )(SeO 4 ) 2 (H 2 O)](H 2 O) 4 (M = Mg, Zn)