Structural features of triarylantimony derivatives Ph3Sb(OC6H3F2-2,4)2 and Ar3Sb[OC(O)R]2 [Ar = Ph, R = CHF2, Ar = 2-MeOC6H4, R = C6H3F2-2,5, Ar = 3-CF3C6H4, R = Ph, Ar = (2-MeO)(5-Br)C6H3, R = C6H3F2-2,3]

Triarylantimony derivatives Ph3Sb(OC6H3F2-2,4)2 (1) and Ar3Sb[OC(O)R]2 [Ar = Ph, R = CHF2 (2), Ar = 2-MeOC6H4, R = C6H3F2-2,5 (3), Ar = 3-CF3C6H4, R = Ph (4), Ar = (2-MeO)(5-Br)C6H3, R = C6H3F2-2,3 (5)], obtained by the oxidative addition reaction of triarylantimony and phenol or a carboxylic acid in the presence of tert-butyl hydroperoxide in ether, were structurally characterized by X-ray diffraction analysis (XRD). According to the X-ray diffraction data [(1) [C30H21O2F4Sb, M 611.22; monoclinic syngony, symmetry group C2/c; cell parameters: a = 14.790(5), b = 15.914(5), c =12.149(5) Å; β = 114.625(11) deg; V = 2599.4(15) Å3, Z = 4, calc = 1.562 g/cm3,  = 1.116 mm1, F(000) = 1216.0, 2θ data acquisition range, deg: 6.0693.48, crystal size 0.54×0.38×0.25 mm; reflection index ranges –30 ≤ h ≤ 30, –32 ≤ k ≤ 32, –24 ≤ l ≤ 24; total reflections 70946; independent reflections 11678; Rint = 0.0800; GOOF 1.061; R1 = 0.0497, wR2 = 0.0943; residual electron density 0.90/–0.62 e/Å3], (2) [C22H17O4F4Sb, M 543.11; triclinic syngony, symmetry group P–1; cell parameters: a = 9.052(4), b = 10.365(3), c = 12.095(4) Å;  = 86.342(13), β = 72.929(16),  = 83.248(17); V = 1076.7(7) Å3, Z = 2, calc = 1.675 g/cm3,  = 1.341 mm1, F(000) = 536.0, 2θ data acquisition range, deg: 6.0254.3, crystal size 0.35×0.27×0.16 mm; reflection index ranges –11 ≤ h ≤ 11, –13 ≤ k ≤ 13, –15 ≤ l ≤ 15; total reflections 26137; independent reflections 4762; Rint = 0.0242; GOOF 1.094; R1 = 0.0378, wR2 = 0.1043; residual electron density 1.78/–1.53 e/Å3], (3) [C35H27O7F4Sb, M 757.32; triclinic syngony, symmetry group P-1; cell parameters: a = 9.247(5), b = 11.793(8), c = 16.103(14) Å;  = 71.42(3), β = 74.90(3),  = 81.53(2); V = 1603(2) Å3, Z = 2, calc = 1.569 g/cm3,  = 0.932 mm1, F(000) = 760.0, 2θ data acquisition range, deg: 5.8457, crystal size 0.5×0.17×0.04 mm; reflection index ranges –12 ≤ h ≤ 12, –15 ≤ k ≤ 15, –21 ≤ l ≤ 21; total reflections 89464; independent reflections 8123; Rint = 0.0494; GOOF 1.036; R1 = 0.0257, wR2 = 0.0558; residual electron density 0.57/–0.39 e/Å3], (4) [C35H22O4F9Sb, M 799.28; monoclinic syngony, symmetry group P21/n; cell parameters: a = 11.183(5), b = 19.867(7), c = 14.905(6) Å; β = 91.216(16); V = 3311(2) Å3, Z = 4, calc = 1.604 g/cm3,  = 0.922 mm−1, F(000) = 1584.0, 2θ data collection range, deg: 6.1−54.26, crystal size 0.41×0.37×0.2 mm; reflection index ranges –14 ≤ h ≤ 14, –25 ≤ k ≤ 25, –19 ≤ l ≤ 19; total reflections 50654; independent reflections 7304; Rint = 0.0308; GOOF 1.014; R1 = 0.0379, wR2 = 0.0974; residual electron density 1.33/–1.14 e/Å3], (5) [C35H24O7F4Br3Sb, M 994.02; triclinic syngony, symmetry group P–1; cell parameters: a = 9.568(10), b = 11.554(11), c = 17.496(16) Å;  = 73.52(3), β = 86.06(3),  = 86.93(7); V = 1849(3) Å3, Z = 2, calc = 1.785 g/cm3,  = 4.053 mm1, F(000) = 964.0, 2θ data acquisition range, deg: 5,7450,34, crystal size 0,3×0,15×0,05 mm; reflection index intervals –11 ≤ h ≤ 11, –13 ≤ k ≤ 13, –20 ≤ l ≤ 20; total reflections 27447; independent reflections 6557; Rint = 0.0676; GOOF 1.019; R1 = 0.0470, wR2 = 0.1033; residual electron density 1.52/–1.48 e/Å3] in crystals of complexes 1–5, the antimony atoms have a distorted trigonal-bipyramidal coordination with the oxygen atoms in axial positions. Taking into account the coordination of the carbonyl oxygen atoms of carboxyl ligands with the central metal atom in compounds 2–5, in which the Sb O(=C) distances are significantly lower than the sum of the covalent radii of the partner atoms, we can speak of an increase in the CN of the antimony atom to 7. In complexes 3 and 5, containing potential coordinating centers (the oxygen atoms of methoxy groups) in the ortho positions of the aryl substituents, the CN of the central metal atom increases to 10. Complete tables of atomic coordinates, bond lengths, and bond angles have been deposited in the Cambridge Structural Data Bank (No. 2217062 (1), 2332595 (2), 2223829 (3), 2331477 (4), 2233172 (5); deposit@ccdc.cam.ac .uk; https://www.ccdc.cam.ac.uk).