Hydroxystibonium Complexes: [(2,6-(OMe)2C6H3)3SbOH]I and [(2,6-(OMe)2C6H3)3SbOH]ClO4·0.5EtOH Synthesis and Structure

Hydroxystibonium complex [(2,6-(OMe)2C6H3)3SbOH]I (I) was obtained by recrystallization of the product of iodination of tris(2,6-dimethoxyphenyl)stibine from wet pyridine. The reaction of benzene solutions of tris(2,6-dimethoxyphenyl)antimony dibromide and silver perchlorate followed by recrystallization from ethanol afforded complex [(2,6-(OMe)2C6H3)3SbOH]ClO4·0.5EtOH (II) with a similar antimony organic cation. Comparative characterization of the compounds was carried out using IR spectroscopy and X-ray diffraction methods. According to X-ray diffraction data (CCDC nos. 2 556 559 (I), 2 556 560 (II)), the tetrahedral [(2,6-(OMe)2C6H3)3SbOH]+ cations of the compounds have a structural similarity. The OSbC bond angles are 101.8(1)°–112.1(1)° (I), 98.3(1)°–110.6(1)°, 97.1(1)°–110.3(1)° (II); the CSbC angles are 104.8(1)°–115.1(1)° (I), 108.2(1)°–114.7(1)°, 105.3(1)°–118.2(1)° (II). The Sb–O and Sb–C interatomic distances are 1.910(3) Å (I), 1.914(3), 1.918(3) Å (II); and 2.073(3)–2.080(3) Å (I), 2.074(4)–2.089(3), 2.072(4)–2.083(4) Å (II).