Two isomeric tridecafluoridotetrabromate(III) anions, [Br₄F₁₃]^–, both previously predicted by quantum‐chemical calculations, have serendipitously been obtained from the reaction of BrF₃ with BaF₂. Single crystals of Ba₂[Br₃F₁₀]₂[Br₄F₁₃]₂ were selected from the reaction mixture at approximately 10 °C. The crystal structure contains two novel, isomeric [Br₄F₁₃]^– anions besides the known, star‐shaped [Br₃F₁₀]^– anions. It crystallized in the monoclinic space group P1n1 (No. 7) with a = 8.8519(18), b = 15.217(3), c = 14.628(3) Å, β = 90.34(3)°, V = 1970.4(7) ų and Z = 2, mP124 at 100 K. The compound was additionally investigated using quantum‐chemical solid‐state calculations. If however crystals from the above reaction mixture were selected at room temperature, the compound Ba[Br₃F₁₀]₂·BrF₃ was obtained containing disordered BrF₃ molecules of crystallization besides [Br₃F₁₀]^– anions. The [Br₄F₁₃]^– molecules were no longer present. Ba[Br₃F₁₀]₂·BrF₃ crystallized in the cubic space group Pa3 (No. 205) with a = 12.4903(14) Å, V = 1948.6(7) ų, Z = 4, cP124, T = 100 K. The much easier to handle latter compound was additionally investigated using powder X‐ray diffraction, as well as IR and Raman spectroscopy.

中文翻译：

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固态中两种量子化学预测的同构[Br4F13] –阴离子的制备

从BrF ₃与BaF ₂的反应中偶然获得了两个同位的十三氟代_四溴酸酯（III）阴离子[Br ₄ F ₁₃ ] ^–。在约10℃下从反应混合物中选择Ba ₂ [Br ₃ F ₁₀ ] ₂ [Br ₄ F ₁₃ ] _2的单晶。晶体结构除包含已知的星形[Br ₃ F ₁₀ ]外，还包含两种新型的异构体[Br ₄ F ₁₃ ] ^–阴离子。] ^–阴离子。它在单斜空间群P 1 n 1（第7号）中结晶，a = 8.8519（18），b = 15.217（3），c = 14.628（3）Å，β = 90.34（3）°，V = 1970.4 （7）一种³和ž = 2，的mP 124在100 K.使用量子化学固态计算该化合物另外调查。然而，如果在室温下从上述反应混合物中选择晶体，则获得的化合物Ba [Br ₃ F ₁₀ ] ₂ · BrF ₃含有无序的BrF _3。[Br ₃ F ₁₀ ] ^–阴离子以外的结晶分子。[Br ₄ F ₁₃ ] ^–分子不再存在。巴[BR ₃ ˚F ₁₀ ] ₂ · BRF ₃结晶立方空间群帕3与（205号）一个= 12.4903（14）A，V = 1948.6（7）³，Ž = 4，厘泊124，Ť = 100K。使用粉末X射线衍射以及IR和拉曼光谱对另外一种较易处理的化合物进行了研究。