Synthesis and structure of the reaction product of penta-para-tolyl antimony with heptafluoropropyl(t-butyl)diketone-1,3 p-Tol4Sb[t-BuC(O)СHС(О)С3F7]

Penta( para -tolyl)antimony reacts with heptafluoropropyl( t -butyl)diketone-1,3 with the splitting out of toluene and formation of the substitution product p -Tol4Sb[ t -BuC(O)СHС(О)С3F7] (1), yielding 82%. The compound was identified by IR spectroscopy and X-ray diffraction analysis. The X-ray analysis was performed on an automatic four-circle diffractometer D8 Quest Bruker (MoKa radiation, λ = 0.71073 Å, graphite monochromator) at 293 K. Crystal size is 0.59 × 0.48 × 0.13 mm, P -1, a = 10.47(2), b = 10.94(2), c = 17.04 (3) Å, α = 73.12 (6), β = 88.94(8), γ = 89.94(8) deg., V = 1867 (7) Å3, Z = 2, ρ = 1.39 g/cm3, F (000) = 792.0, the 2θ interval is 3.89-56.999 deg., R 1 = 0.2213, wR 2 = 0.5429. According to the X-ray diffraction data, compound 1 is a molecular complex, in which the antimony atoms have an octahedral coordination with two oxygen atoms and two carbon atoms in the equatorial plane; the axial positions are occupied by the two remaining tolyl ligands. The CSbC axial angle is strongly distorted and is equal to 159.6 (8)°. The CSbO diagonal angles in the equatorial plane are 167.1(7)°, 166.9(7)°. The lengths of the Sb-C bonds are 2.11(2) and 2.19 (3) Å. The formation of the chain spatial structure of crystals is due to formation of bonds between the molecules involving fluorine (H∙∙∙F 2.64-2.83 Å) and carbon (C∙∙∙F 3.005 Å) atoms. Complete tables of atomic coordinates, bond lengths, and valence angles are deposited in the Cambridge Structural Data Bank (No. 2067768 (1); deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk/data_request/cif).