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Extracting residues of an aqueous solutions containing equimolar amounts of K[C(CN) 3 ] and RbF or CsF, respectively, with absolute ethanol, yields triangular, transparent colorless crystals of Rb[C(CN) 3 ] and Cs[C(CN) 3 ] after the ethanol was allowed to evaporate. The compounds are isotypic and crystallize isopointal to calcite in space group  R 3̅ c  (no. 167) with the cell parameters  a =809.9(1) and  c =1461.3(3) pm and  a =843.29(9) and  c =1459.9(2) pm, respectively. Single crystals were used to record the Raman spectra of the title compounds.

Syntheses, single-crystal structure determination, and Raman spectra of Rb[C(CN) 3 ] and Cs[C(CN) 3 ]