Triphenylbismuth dicarboxylate Ph3BiOC (O) C6H3F2-2, 32 was synthesized by an oxidative addition reaction between triphenylbismuth and 2, 3-difluorobenzoic acid in the presence of tert-butyl hydroperoxide in diethyl ether. The compound was identified by IR spectroscopy and X-ray diffraction analysis. According to X-ray diffraction data, the bismuth atoms in the crystals of the compound C32H21O4F4Bi, FW is 754. 47; triclinic system, space group P 1 ; cell parameters: a = 9. 023 (4) Å, b = 11. 208 (4) Å, c = 14. 784 (6) Å; α = 70. 166 (13) °, β = 86. 68 (3) °, γ = 82. 698 (14) °; V = 1394. 9 (10) Å3; crystal size 0. 36 × 0. 14 × 0. 09 mm; index ranges –15 ≤ h ≤ 15, –18 ≤ k ≤ 19, –25 ≤ l ≤ 25; total reflections 91 795; independent reflections 14 244; Rint 0. 0426; GOOF 1. 010; R1 = 0. 0315, wR2 = 0. 0613; residual electron density 1. 12/–0. 91 e/Å3 have a distorted trigonal bipyramidal coordination with the oxygen atoms of the carboxylate ligands in axial positions (the axial angle is 172. 19 (6) °). The sum of the CBiC bond angles in the equatorial plane is 359. 92 (9) °. The Bi–O distances are 2. 291 (2) and 2. 250 (2) Å, the Bi–C bond lengths vary in the range 2. 193 (3) –2. 216 (2) Å. The bismuth atom deviates from of the equatorial plane C3 by 0. 033 Å. In the structure of the compound, Bi⋅⋅⋅O (=C) intramolecular contacts are observed, which is significantly less than the sum of the van der Waals radii of Bi and O atoms (3. 9 Å). The spatial crystal structure of the compound is formed due to the presence of hydrogen bonds such as H⋅⋅⋅O (=C), H⋅⋅⋅F, and CH⋅⋅⋅π interactions. Atomic coordinates, bond lengths, and bond angles have been deposited in the Cambridge Crystallographic Data Center (CCDC no. 1981641; deposit@ccdc. cam. ac. uk; https: //www. ccdc. cam. ac. uk).
Efremov et al. (Wed,) studied this question.