Abstract

The interaction of antimony iodide with iodides of n-pentyltriphenylphosphonium (1 : 1 mol.) in acetone and tetraphenylphosphonium (3 : 2 mol.) in 2-ethoxyethanol yielded [n-C₅H₁₁PPh₃]₂ [Sb₂I₈(acetone)₂] and [Ph₄P]₃[Sb₂I₉] ∙ EtO(CH₂)₂OH ionic complexes, whose structures were established using X-ray diffraction analysis. According to the XRD data, phosphorus atoms in cations have slightly distorted tetrahedral coordination with CPC bond angles of 107.48(11)°−111.52(11)° and 106.5(3)°−113.3(3)° and close P−C 1.795(3)−1.802(2) Å and 1.787(5)−1.809(6) Å bond lengths in 1 and 2, respectively. In the centrosymmetric [Sb₂I₈(acetone)₂]^2– anion, antimony atoms have a distorted octahedral coordination (trans-angles of 171.476(9)–176.33(3)°; the acetone molecule occupies an axial position coordinated by the oxygen atom (Sb∙∙∙O of 2.820(10) Å). Sb–I_bridge bonds (3.0997(12) Å) are longer than Sb–I_term bonds (2.7780(8)–2.9553(10) Å). In the [Sb₂I₉]^3– anion, ISbI trans-angles vary in the 169.612(17)°–173.426(19)° range; the Sb–I_term bonds (2.8613(13)–2.9609(12) Å) are shorter than Sb–I_bridge bonds (3.0986(12)–3.2760(13) Å). 2-Ethoxyethanol solvate molecules form dimers via O(1)∙∙∙H(2A) hydrogen bonds of 2.11 Å. The complete tables of the atomic coordinates, bond lengths, and bond angles for the structures were deposited at the Cambridge Crystallographic Data Center (no. 1984511 (1), no. 2157456 (2); deposit@ccdc.cam.ac.uk; https://www.ccdc.cam.ac.uk).

中文翻译：

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[n-C5H11PPh3]2[Sb2I8(丙酮)2] 和 [Ph4P]3[Sb2I9] ∙ EtO(CH2)2OH 锑配合物的合成和结构

摘要

碘化锑与丙酮中的正戊基三苯基鏻 (1:1 摩尔) 和 2-乙氧基乙醇中的四苯基鏻 (3:2 摩尔) 的碘化物相互作用，生成 [ n -C ₅ H ₁₁ PPh ₃ ] ₂ [Sb ₂ I ₈ (丙酮) ₂ ] 和 [Ph ₄ P] ₃ [Sb ₂ I ₉ ] ∙ EtO(CH ₂ ) ₂OH 离子配合物，其结构是通过 X 射线衍射分析确定的。XRD数据显示，阳离子中的磷原子具有轻微扭曲的四面体配位，CPC键角为107.48(11)°−111.52(11)°和106.5(3)°−113.3(3)°，接近P−C 1.795( 1和2中的键长分别为 3)−1.802(2) Å 和 1.787(5)−1.809(6) Å 。在中心对称的[Sb ₂ I ₈ (丙酮) ₂ ] ^2–阴离子中，锑原子具有扭曲的八面体配位（反角为171.476(9)–176.33(3)°；丙酮分子占据由氧原子（2.820(10) Å 的 Sb∙∙∙O）。Sb-I_桥键 (3.0997(12) Å) 比 Sb-I_项键 (2.7780(8)–2.9553(10) Å) 长。在[Sb ₂ I ₉ ] ^3–阴离子中，ISbI反式角在169.612(17)°–173.426(19)°范围内变化；Sb-I_端键 (2.8613(13)–2.9609(12) Å) 比 Sb-I_桥键 (3.0986(12)–3.2760(13) Å) 短。2-乙氧基乙醇溶剂化物分子通过 2.11 Å 的 O(1)∙∙∙H(2A) 氢键形成二聚体。结构的原子坐标、键长和键角的完整表存放在剑桥晶体学数据中心（编号 1984511 ( 1 )、编号 2157456 ( 2 )；deposit@ccdc.cam.ac.uk； https://www.ccdc.cam.ac.uk）。