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3SbF3•4SbF5has been prepared from the reaction of SbF3with a large excess of SbF5and from the reaction of WF5with SbF5in Genetron 113. An X-ray structure determination has shown that the compound crystallizes in the monoclinic space group P21/cwith a = 8.547(10), b = 13.521(8), c = 19.551(12) Å, β = 100.3(1)°,Z = 4with the final residual indices of R = 0.0486 and Rw = 0.0526 for 4274 unique reflections. If only Sb—F distances of less than 2.1 Å are considered the structure can be viewed in terms of the arrangement (SbF2+)(SbF2+)(SbF6−)4. A Raman spectrum from single crystals of the compound is reported. Keywords: X-ray, structure, antimony, fluoride, Raman.