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M r = 449.5, monoclinic, C2/c, a = 15.144(3), b=5.890(3), c=10.149(1)A, fl= 102.55 (1) °, V= 883.7 A 3, Z = 4, D x = 3.380 Mg m -3, Mo K~t, 2 = 0.71073/k, /z = 16.58mm -1, F(000)= 832, T=292K, final R = 0.048 for 1006 observed reflections. Trirubidium hydrogenbis(sulfate) is isostructural with its triammonium analogue. The room-temperature structure for these two salts is pseudohexagonal and phase transitions to hexagonal symmetry at elevated temperatures are predicted to involve changes in the O-H-O hydrogen bonds.