Affiliations: Department of Chemistry, Nizhny Novgorod State University, Gagarin av., 23, 603600, Nizhny Novgorod, Russia | G. A. Razuvaev Institute of Organometallic Chemistry, Russian Academy of Sciences, Tropinin str. 49, 603600 Nizhny Novgorod, Russia | N. D. Zelinsky lnstitute of Organic Chemistry, Russian Academy of Sciences, Leninsky prosp., 47, 117913, B-334, Moscow, Russia
Note: [] Corresponding author.
Abstract: The oxidation of triphenylantimony and triphenylphosphine by tert-butylhdroperoxide in the presence of catechol gives a new complex of a hexa-coordinated antimony, (C6H4O2)SbPh3(OPPh3).7 In this complex triphenylphosphine oxide plays the role of the sixth ligand in a coordination sphere of an antimony atom of triphenylantimony o-phenylenedioxide. The compound was characterized by IR, 1H NMR, 13C NMR, 31P NMR and X-ray single-crystal diffraction method. Crystal data for 7 at T = 293 K: a = 21.111(1) Å, b = 13.910(4) Å, c = 25.052(8) Å, β = 96.48(3)°, V = 73104(4) Å3, Z = 8, Dcalc = 1.380 g/cm3, μ = 0.839 mm−1, space group C2/c. The geometry of the antimony atom in the synthesized complex is a distorted octahedron. Sixth coordination Sb-O(P) – 2.33 Å – is comparable with the sum of covalent radii of antimony and oxygen atoms, 2.20 Å. Five analogous complexes containing trimethyl(triethy1)antimony o-phenylenedioxide or 2.2.2-triphenyl-1.3.2-dioxas-tibolane and triphenylphosphine oxide or triphenylantimony o-phenylenedioxide and dimethylsulfoxide or pyridine oxide as a monodentate ligand were synthesized in the same manner. These compounds were also characterized by IR, 1H 13C and 31P NMR.
