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Thermal expansion studies on [N(CH 3 ) 4 ] 3 Sb 2 Cl 9  and [N(CH 3 ) 4 ] 3 Sb 2 Br 9  are reported. The relaxation times  1 H T 1  were measured for [N(CH 3 ) 4 ] 3  Bl 2 Cl 9  , [N(CH 3 ) 4 ] 3 Sb 2  Br 9  , and [N(CH 3 ) 4 ] 3  Bi 2  Br 9  in the temperature range 100-290 K. To interpret the T 1  data on [N(CH 3 ) 4 ] 3 Bi 2 Cl 9  the method of T 1  calculation reported by Takeda et al. has been applied successfully. Two different, inequivalent types of [N(CH 3 ) 4 ] 3  +  cations for all tetramethylammonium crystals are found.

NMR and Dilatometric Studies on [N(CH 3 ) 4 ] 3 M 2 X 9 (M = Sb, Bi; X = Cl, Br)