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The 1:1 and 1:2 phases (TTM -TTF)Br 3  and (TTM -TTF)(Br 3 ) 2 , TTM -TTF = tetra(methylthio)tetrathiafulvalene, C 10 H 12 S 8 , have been crystallized by diffusion of bromine vapour into solutions of the donor. The 1:1 salt is monoclinic, P 2 1 /n, a = 7.587(2), b = 11.424(3), c = 23.145(8) Å , β = 95.80(3)°, V = 1997 Å 3 , Z = 4, M r  = 628.45, d c  = 2.09 g cm -3 , final R w  = 0.028 for 912 reflections. The 1:2 salt is monoclinic, C2/m, a = 11.510(3), b = 17.039(4), c = 9.770(3), β = 141.62(1)°, V = 1190 Å 3 , Z = 2, M r  = 868.16, d c  = 2.42 g cm -3 , final R w  = 0.029 for 899 reflections. Diadic stacks of the monopositive donor cations are found in the 1:1 salt, whereas the dipositive cations in the 1:2 salt form sheets via short intermolecular S···S contacts. A relation between bond lengths and charge is indicated.

Tribromide Salts of the Organic Donor Tetra(methylthio)tetrathiafulvalene, [TTM-TTF] + (Br 3 - ) and [TTM-TTF] 2+ (Br 3 - ) 2