The Synthesis and Structure of [n-C5H11PPh3]2[Sb2I8(acetone)2] and [Ph4P]3[Sb2I9] ∙ EtO(CH2)2OH Antimony Complexes

• Published in: Review journal of chemistry Vol. 13; no. 1; pp. 46 - 52
• Main Authors: Senchurin, V S, Sharutin, V V, Bezhin, V K
• Format: Journal Article
• Language: English
• Published: Heidelberg Springer Nature B.V 2023
• Subjects: Acetone; Anions; Antimony; Chemical bonds; Coordination; Crystallography; Data centers; Hydrogen bonds; Iodides
• ISSN: 2079-9780; 2079-9799
• DOI: 10.1134/S2634827623700174

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–Ibridge bonds (3.0997(12) Å) are longer than Sb–Iterm 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–Iterm bonds (2.8613(13)–2.9609(12) Å) are shorter than Sb–Ibridge 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); [e-mail]; https://www.ccdc.cam.ac.uk).