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A reliable synthesis of unstable and highly reactive BrO2F is reported. This compound can be converted into BrO2+SbF6−, BrO2+AsF6−, and BrO2+AsF6−⋅2 BrO2F. The latter decomposes into mixed‐valent Br3O4⋅Br2+AsF6− with five‐, three‐, one‐, and zero‐valent bromine. BrO2+ H(SO3CF3)2− is formed with HSO3CF3. Excess BrO2F yields mixed‐valent Br3O6+OSO3CF3− with five‐ and three‐valent bromine. Reactions...
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