The crystal structures of RbSb₂F₁₁, TlSb₂F₁₁, O₂Sb₂F₁₁ and β-NH₄Sb₂F₁₁ salts are isotypical and crystallize in the orthorhombic space group Cmc2₁ (No. 36). Crystal data of rubidium salt: a = 19.9981(3) Å, b = 11.5093(2) Å, c = 12.9623(2) Å, V = 2983.46(8) ų, and Z = 12 at 150 K. Unit cell parameters of corresponding thallium salt: a = 19.9876(5) Å, b = 11.5400(3) Å, c = 13.0267(3) Å, V = 3004.70(13) ų and Z = 12 at 150 K. Reaction between NH₄F and excess of SbF₅ in anhydrous HF resulted in the single-crystal growth of β-NH₄Sb₂F₁₁: a = 20.0406(7) Å, b = 11.5534(4) Å, c = 13.0796(4) Å, V = 3028.42(18) ų, and Z = 12 at 296 K. The XRD experiments on NH₄Sb₂F₁₁ at 240 and 150 K revealed another modification (α-NH₄Sb₂F₁₁), which crystallizes in a (pseudo-hexagonal) monoclinic cell, space group P2₁, a = 11.5045(6) Å, b = 13.0437(3) Å, c = 11.5264(6) Å, β = 119.818(7)°, V = 1500.67(15) ų, and Z = 6 at 240 K. Reaction between the O₂SbF₆ and SbF₅ in anhydrous HF yielded O₂Sb₂F₁₁ upon crystallization with a = 19.8472(5) Å, b = 11.1172(3) Å, c = 12.8259(3) Å, V = 2829.97(12) ų, and Z = 12 at 150 K. The crystal structures of ASb₂F₁₁ (A = Rb⁺, Tl⁺, O₂⁺, NH₄⁺) salts consist of dimeric Sb₂F₁₁⁻ anions with partially disordered terminal fluorine atoms. Negative charge of the anions is compensated by single charged cations. Crystal structure of α-NH₄Sb₂F₁₁ demonstrates similar motif as in β-phase but with slightly re-arranged N―H… F hydrogen bonds. In the 100−296 K range, only rhombohedral phase was observed for NH₄SbF₆ (rhombohedral space group R $\overline{3}$, No. 148) with a = b = 7.5961(9) Å, c = 7.7176(9) Å, α = β = 90°, γ = 120°, V = 385.65(12) ų, and Z = 3 at 150 K).

RbSb ₂ F ₁₁，TlSb ₂ F ₁₁，O ₂ Sb ₂ F ₁₁和β- NH ₄ Sb ₂ F ₁₁盐的晶体结构是同型的，并且在正交晶空间群Cmc2 ₁（第36号）中结晶。铷盐的晶体数据：一个 = 19.9981（3）埃，b  = 11.5093（2）埃，c ^  = 12.9623（2），V  = 2983.46（8）埃³，与ž  = 12个，在150个K.晶胞参数对应铊盐：一个 = 19.9876（5），b  = 11.5400（3）埃，c ^  = 13.0267（3）A，V  = 3004.70（13）一种³和Ž  = 12在NH之间150 K.反应₄ F和过量的SbF的₅在无水HF导致β - NH ₄ Sb ₂ F ₁₁的单晶生长：a  = 20.0406（7）Å，b  = 11.5534（4）Å，c  = 13.0796（4）Å，V  = 3028.42（18）Å ³， 在296 K时Z =12。在NH ₄ Sb ₂ F ₁₁上的XRD实验在240和150 K时揭示了另一种修饰（α- NH ₄ Sb ₂ F ₁₁），其在一个（伪六边形）单斜晶胞空间群P2 ₁中结晶，a  = 11.5045（6）Å，b  = 13.0437（3）埃，ç  = 11.5264（6）A，β  = 119.818（7）°，V  = 1500.67（15）一种³，和ž  = 6在将O之间240 K.反应₂的SbF ₆和的SbF ₅在无水HF，得到ö ₂的Sb ₂ ˚F ₁₁在与结晶一 = 19.8472（5），b  = 11.1172（3）埃，c ^  = 12.8259（3）A，V  = 2829.97（12）一种³，和ž  = 12，在150 K的ASB的晶体结构₂ ˚F ₁₁ A（ = RB ⁺，铊⁺，O- ₂ ⁺，NH ₄ ⁺）盐包括二聚的Sb ₂ ˚F ₁₁ ^-具有部分无序终端氟原子的阴离子。阴离子的负电荷由单电荷阳离子补偿。α- NH ₄ Sb ₂ F _11的晶体结构表现出与β相相似的基序，但N-H…F氢键稍微重排。在100-296 K范围内，仅观察到NH ₄ SbF _6的菱面体相（菱面体空间群R $\overline{3}$148号）与一个= b  = 7.5961（9）埃，c ^  = 7.7176（9）埃，α = β  = 90°，γ  = 120°，V  = 385.65（12）一种³，和ž  = 3在150 K）。