Gallium-69 and -71 and indium-115 n.m.r. spectra have been obtained for the tetrahalometallate anions MX4- (M = Ga, In; X = Cl, Br, I) in dichloromethane solution. For each element, mixtures of two halo anions gave mixed halo species in the statistical distribution. For gallium, a mixture of the three halo anions gave all 15 possible species in the statistical distribution. The effect of the electric quadrupole moment is clearly reflected in the linewidths; gallium-71 gave sharper lines and better resolution of the mixed species than gallium-69 and the resonances for indium-1 15 were very broad.