The ratio of the anisotropic magnetic susceptibility r χ [ ð 2 À 3 Þ=ð 1 À 2 Þ] of a biaxial crystal was determined using a suspension of its microcrystalline powder. The suspension was rotated in a static magnetic field and subjected to in situ X-ray diffraction measurement. Following the theory proposed previously to relate the X-ray half-widths to the orientation fluctuation, the experimentally obtained half-widths were translated to the orientation fluctuation that is relevant to the magnetic anisotropy 2 À 3 , 1 À 3 , and 1 À 2 . L-Alanine and D-mannitol microcrystals were investigated and their r χ values were determined as 1.0 and 1.2, respectively, which were in good agreement with those reported in the literature. By using the determined r χ value of L-alanine, it was demonstrated that this value is a crucial parameter for determining the experimental magnetic condition when preparing a three-dimensional magnetically oriented microcrystal array that produces high-quality X-ray diffractions.