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Transparent colorless crystals of Na A  5 [C 6 N 9 ] 2  · 4 H 2 O ( A  = Rb, Cs) were obtained by blending aqueous solutions of Na 3 [C 6 N 9 ] and RbF or CsF, respectively, and subsequent evaporation of the water under ambient conditions. Both compounds crystallize in the space group  P 2 1 / m  (no. 11) with the cell parameters  a  = 815.56(16),  b  = 1637.7(4) and  c  = 1036.4(3) pm, and  β  = 110.738(12)° for NaRb 5 [C 6 N 9 ] 2  · 4 H 2 O and  a  = 843.32(6),  b  = 1708.47(11) and  c  = 1052.42(7) pm, and  β  = 112.034(2)° for NaCs 5 [C 6 N 9 ] 2  · 4 H 2 O, respectively. Raman spectra of the title compounds complement our results.

Synthesis, single-crystal structure determination and Raman spectra of the tricyanomelaminates Na A 5 [C 6 N 9 ] 2 · 4 H 2 O ( A = Rb, Cs)