Synthesis of tetraphenylantimony 3-fluorophenylacetate from pentaphenylantimony and triphenylantimony bis(3-fluorophenyl acetate)

The interaction of equimolar amounts of pentaphenylantimony and bis (3-fluorophenylacetato)triphenylantimony in benzene yielded 92% tetraphenylantimony 3-fluorophenylacetate (1), which was identified by IR spectroscopy and X-ray structural analysis. X-ray diffraction analysis was performed on a D8 QUEST diffractometer from Bruker. The crystallographic characteristics of the unit cell of the compound are as follows: monoclinic space group C c, a = 10,2427(6), b = 17,7825(7), c = 14,6472(5) Å, β = 95,260(4), V = 2656,60(17) Å3, Z = 4, ρcalc = 1,458 g/cm3, m = 1,072 mm-1, F(000) = 1176,0, crystal size 0,32´0,2´0,09 mm, data collection range for 2θ, deg: 6,952-56,992, index range -13 ≤ h ≤ 12, -19 ≤ k ≤ 23, -19 ≤ l ≤ 19, number of measured reflections 9906, number of independent reflections 4334, R int = 0,0228, GOOF = 1,139, number of parameters 330, R 1 = 0,0350, wR 2 = 0,1042. According to X-ray diffraction data, the antimony atoms in the compound have a distorted trigonal-bipyramidal coordination with the oxygen atom of the carboxylate group in the axial position. The axial angle CSbO is 175,9(2)º. The sum of the equatorial angles CSbC is 357,1(9)°, the Sb-Ceq distances [2,109(7), 2,117(5), 2,146(5) Å] are significantly shorter than the Sb-Cax [2,194(7) Å] and Sb-O [2,244(4) Å] bond lengths. The organization of molecules in the crystal of compound 1 is due to hydrogen bonds and CH∙∙∙π-interactions of the rings of the aryl and carboxyl ligands. Complete tables of atomic coordinates, bond lengths, and bond angles have been deposited with the Cambridge Crystallographic Data Center (No. 2055555; deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk/data_request/cif).