A pseudo single crystal (a composite of matrix resin and powder crystallites, wherein the individual crystallites are aligned three‐dimensionally) was prepared from a powder of sucrose, and its X‐ray diffraction pattern was studied. A powder of sucrose crystals suspended in a UV‐curable resin precursor was subjected to magnetic alignment in order to align the individual crystallites three‐dimensionally, and then the resin precursor was photopolymerized to maintain this orientation. The pseudo single crystal thus obtained produced a well resolved X‐ray diffraction profile that is similar to that produced by a twin crystal. The origin of the twin orientation was explained in terms of the interplay between the symmetry of magnetic susceptibility axes and the crystal symmetry (point group 2) of sucrose. The crystal structure of sucrose solved using the pseudo single crystal was in excellent agreement with that solved using a single crystal.
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