In-situ small-angle neutron scattering was performed on Ni-(10 to 12) at.% Ti polycrystals and single crystals at temperatures between 870 and 1270 K. During decomposition metastable precipitates of cuboidal shape form with preferred alignement along <100>. The Ti concentration of these precipitates is 17(1) at.% (between 870 and 950 K). Metastable precipitates precede the formation of platelets of the stable η phase even outside the hitherto accepted metastable miscibility gap.