Synthesis and Structure of the Reaction Product of Penta-para-tolyl antimony with Heptafluoropropyl(t-butyl)diketone-1,3 p-Tol4Sb[t-BuC(O)CHC(O)C3F7]
Abstract
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., R1 = 0.2213, wR2 = 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).
