Electrocrystallization and structures of perylene radical salts: hexaperylene perchlorate, (C20H12)6+ClO4-, triperylene perchlorate, (C20H12)3+ClO4-, and diperylene hexafluorophosphate-tetrahydrofuran (3/2), (C20H12)2+PF6-.2/3C4H8O
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Crystals grown by electrocrystallization, species obtained depending on perylene concentration. Room-temperature data collect ions, Mo Kat λ = 0·71069 A. 6:1 salt: Mr= 1613·3, triclinic. pl, a = 12·57 1 (7), b = 13·699(5). c = 13.835(II)A, α = 110·43 (4), β= 107·13 (7), γ= 107·09 (4)°, V = 1913A3, Z = 1, Dx = 1.40gcm-3, μ= 1.1 cm- ', F(OOO) = 841, final R = 0·077 for 3171 observed reflections. The structure contains three independent perylene π dimers arranged nearly perpendicularly to each other. The anions are severely disordered or freely rotating. 3:1 salt: Mr = 856·4, triclinic, PI, a = 13·009(8), b= 13.821 (10), c= 13·850(15)A, α = 66·05(7), β = 83·36 (8). γ= 63·5 1 (6)°, V = 2030A3, Z = 2, Dx= 1.40gcm-3 , μ= 1·5cm-1 , F(OOO) = 890, final R = 0· 138 for 3523 observed reflections. Tetrameric perylene stacks are surrounded on four sides by single perylene species, having their planes nearly perpendicular to the molecular planes in the stacks. 2:1 salt: Mr = 697· 7, monoclinic, P2/m, a = 13·04(1), b = 14 · 12 (1), c = 13·75 (1)A, β=110·80 (2)°, V = 2367 A3, Z = 3, Dx = 1·47 g cm-3',μ= 1·5 cm- ', F(OOO) = 1079, final R =0· 121 for 1737 observed reflections. Nearly regular perylene stacks are surrounded by single perylene species in a way similar to the 3:1 salt. The thf solvent and one of the perylene molecules are disordered over two orientations.