Synthesis and structure of 1,1,1,5,5,6,6,6-осtafluorohexane-2,4-dionato-tetraphenylantimony

Abstract

Heating a benzene solution of equimolar amounts of pentaphenylantimony and 1,1,1,5,5,6,6,6-octafluorohexane-2,4-dione in a sealed ampoule followed by slow cooling resulted in the formation of tetraphenylantimony β-diketonate Ph4Sb[CF3CF2C(O)CHC(O)CF3] (1) with a yield of 87%, the structure of which was proven by X-ray structural analysis. X-ray diffraction analysis was performed on a D8 Quest Bruker automated four-circle diffractometer (Mo Kα radiation, λ = 0,71073 Å, graphite monochromator) at 293 K. Crystals (1) C60H42O4F16Sb2 (M 1374,49 g/mol): triclinic, space group P–1, a 11,315(5) Å, b 16,152(7) Å, c 16,823(9) Å, α 75,460(19)°, β 78,89(3)°, γ 89,639(18)°, V 2918(2) Å3, Z 2, μ = 1,022 mm–1, ρcalc = 1,5644 g/cm3, 147353 reflections measured, 16829 independent reflections (Rint 0,0718), number of refined parameters 739, GOOF 0,946, R-factors for F2 > 2σ(F2) R1 0,0731, wR2 0,2172, R-factors for all reflections R1 0,1259, wR2 0,2860. The crystal contains two types of crystallographically independent molecules a, b. The antimony atom in molecule 1 is hexacoordinated, the equatorial positions contain carbon and oxygen atoms, and the axial positions contain two carbon atoms of phenyl radicals.