The structure study of tris(4-fluorophenyl)antimony dicarboxylates (4-FC6H4)3Sb[OC(O)R]2(R=C6H3F2-2,3, C6H3(NO2)2-3,5, C6H4OMe-2,CF2Br, CH=CHPh,CH3, C?CH)

The interaction of tris(4-fluorophenyl)antimony with 2,3-difluorobenzoic acid, as well as with 3,5-dinitrobenzoic, 2-methoxybenzoic, bromodifluoroacetic, cinnamic, formic, and propionic acids in the presence of tert-butyl hydroperoxide (1:2:1 mol.) in ether at ambient temperature has given tris(4-fluorophenyl)antimony dicarboxylates (4-FC6H4)3Sb[OC(O)R]2, where R = C6H3F2-2,3 (1), C6H3(NO2)2-3,5 (2), C6H4OMe-2 (3), CF2Br (4), CH=CHPh (5), CH3 (6), и C≡CH (7). The IR spectra of compounds 1-7, recorded on a Shimadzu IRAffinity-1S Fourier transform IR spectrometer, in a KBr pellet within the 4000-400 cm-1 interval, contain absorption bands of carbonyl groups, which are shifted to the low-frequency vibration region in comparison with the IR spectra of the initial acids. According to the X-ray diffraction data obtained on a Bruker D8 QUEST diffractometer, compound 1 has the following crystallographic parameters of the unit cell: space group P-1, a = 9.034(4), b = 11.351(8), c = 14.814(9) Å, α = 70.11(3)°, β = 88.60(2)°, γ = 87.03(2)°, V = 1426(15) Å3, ρcalc = 1.679 g/cm3, Z = 2. The antimony atom in 1 has a distorted trigonal-bipyramidal coordination with carboxylate ligands in axial positions. The OSbO axial angle is 176.95 (6)°. The lengths of the Sb-O and Sb-C bonds are equal to 2.135(2), 2.121(2) and 2.113(3)-2.116 (3) Å. The Sb···O=C distances are 3.040(2), 2.861 (3) Å, that is, less than the sum of the van der Waals radii of antimony and oxygen (3.70 Å). The antimony atom departs from the equatorial plane [C3] by 0.038 Å. Complete tables of atom coordinates, bond lengths and valence angles are deposited at the Cambridge Crystallographic Data Center (№ 2051716; deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk/data_request/cif).