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A new double lithium rubidium sulphate, Li 3 Rb(SO 4 ) 2  · H 2 O, was found. Single crystals were obtained by  drowning out  in a tetramethoxysilane gel medium. The compound crystallises in the space group  P 1 with parameters  a  = 5.1356(4) Å,  b  = 4.9853(4) Å, and  c  = 8.2712(9) Å,  α  = 90.032(7)°,  β  = 105.729(6)°,  γ  = 90.004(7)° and  Z  = 1. The crystal structure was determinated by X-ray diffraction; in addition the new double sulphate was characterized by IR-spectroscopy. The system Rb 2 SO 4 –Li 2 SO 4 –H 2 O at 323 K is given.

Growth and characterization of the new double sulphate, Li 3 Rb(SO 4 ) 2 · H 2 O