Synthesis and structure of tris(3-fluorophenyl) antimony bis(2,5-dimethylbenzenesulphonate) and bis(dibromofluoroacetate)

The interaction of tris (3-fluorophenyl)antimony with 2,5-dimethylbenzenesulfonic or dibromofluoroacetic acid in diethyl ether in the presence of tert -butyl hydroperoxide has synthesized tris (3-fluorophenyl)antimony bis (2,5-dimethylbenzenesulfonate) (1) and tris (3-fluorophenyl)antimony bis (dibromofluoroacetate) (2). The X-ray diffraction pattern has been obtained at 293 K on an automatic diffractometer D8 Quest Bruker (Mo Kα -radiation, λ = 0.71073 Å, graphite monochromator) for crystal 1 [C34H30F2O6S2Sb, M 777.45, the triclinic syngony, the symmetry group P -1; cell parameters: a 10.634(18) Å, b 11.38(2) Å, c 14.31(3) Å, α = 90.51(8) degrees, β = 90.35(11) degrees, γ = 112.79(5) degrees; V = 1596(5) Å3; the crystal size is 0.5×0.48×0.17 mm; intervals of reflection indexes are -15 ≤ h ≤ 14, -15 ≤ k ≤ 15, -19 ≤ l ≤ 19; total reflections 30473; independent reflections 8318; Rint 0.0920; GOOF 1.894; R1 = 0.1699, wR 2 = 0.4237; residual electron density 6.78/-5.48 e/Å3] and crystal 2 [C22H12O4F7SbBr2, M 754.89, the triclinic syngony, the symmetry group P -1; cell parameters: a 8.98(3) Å, b 10.41(2) Å, c 14.92(3) Å, α = 90.77(7) degrees, β = 90.73(9) degrees, γ = 113.95(10) degrees; V = 1275(5) Å3; the crystal size is 0.65 × 0.32 × 0.14 mm; intervals of reflection indexes are -13 ≤ h ≤ 13, -15 ≤ k ≤ 14, -21 ≤ l ≤ 21; total reflections 61066; independent reflections 8511; Rint 0.0863; GOOF 1.983; R1 = 0.1529, wR 2 = 0.4647; residual electron density 4.41/-3.48 e/Å3] the antimony atoms have a distorted trigonal-bipyramidal coordination. The axial OSbO angles are 178.2(3)° (1) and 174.0(4)° (2); the sum of the CSbC angles in the equatorial plane is 360°. The Sb-O and Sb-C bond lengths are 2.108(9)-2.131(12) Å and 2.090(14)- 2.21(3) Å. The structural organization of crystals 1 and 2 is controlled by intermolecular bonds O···H 2.53-2.70 Å (1) and 2.57-2.60 Å (2), F···H 2.46-2.59 Å (1) and Br···H 3.02 Å (2). In 2 the short contacts C··· F have been observed between the aryl ligands of neighboring molecules 3.079 and 3.085 Å. Complete tables of coordinates of atoms, bond lengths and valence angles for structures 1 and 2 are deposited at the Cambridge Structural Data Bank (no. 2055553, 2055764; deposit@ccdc.cam.ac.uk; http: //www.ccdc.cam.ac.uk).