Two uranyl sulfate hydrates, (H 3 O) 2 [(UO 2 ) 2 (SO 4 ) 3 -(H 2 O)]·7H 2 O (NDUS) and (H 3 O) 2 [(UO 2 ) 2 (SO 4 ) 3 (H 2 O)]·4H 2 O (NDUS1), and one uranyl selenate-selenite [C 5 H 6 N][(UO 2 )(SeO 4 )-(HSeO 3 )] (NDUSe), were obtained and their crystal structures solved.NDUS and NDUSe result from reactions in highly acidic media in the presence of l-cystine at 373 K. NDUS crystallized in a closed vial at 278 K after 5 days and NDUSe in an open beaker at 278 K after 2 weeks. NDUS1 was synthesized from aqueous solution at room temperature over the course of a month. NDUS, NDUS1, and NDUSe crystallize in the monoclinic space group P2 1 /n, a = 15.0249(4) Å, b = 9.9320(2) Å, c = 15.6518(4) Å, β = 112.778(1)°, V = 2153.52(9) Å 3 , Z = 4, the tetragonal space group P4 3 2 1 2, a = 10.