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This paper reports the results of X-ray powder diffraction experiments on C60Br24(Br2)2. This material is a C60 derivative and shows rhombohedral symmetry at room temperature. At low temperature, a rhombohedral-to-triclinic phase transition can be observed that involves a large distortion of the cell while the volume of the unit cell remains almost constant. This is a sufficiently complicated system that high-resolution synchrotron data and a combination of different tactics were required to reach a structure solution.