Evaporation of mixed solution of 2,4,6-tris(4-tert-butylphenyl)phenoxyl 1 M and its phenol analogue 1 OH yielded a solid solution (III), where 1 OH : 1 M = 0.70 : 0.30, which was isomorphic to crystal of 1 OH (II). In contrast, slow evaporation of 1 M concomitant with gradual decomposition giving 1 OH yielded crystal-glass composite (IV) consisting of 1 OH : 1 M with a molar ratio of 0.40 : 0.60. The outer crystal region of IV was attributed to solid solution of 1 OH and 1 M , while the inner glassy region to amorphous consisting of 1 M and its dimer 1 D (I).