Structural features of tris(2-metoxy-5-bromophenyl)antimony bis[2,5-difluorobenzoate] solvate with benzene and octane [(2-MeO)(Br-5)C6H4]3Sb[OC(O)C6H3F2-2,5]2 • 1/2 PhH • 1/2 C8H18 and tri(para-tolyl)antimony bis[2-furancarboxylate] (4-MeC6H4)3Sb[OC(O)C4H3O]2

The structure of tris[(2-methoxy)(5-bromophenyl)antimony] bis[2,5-difluorobenzoate] solvate [(2-MeO)(Br-5)C6H4]3Sb[OC(O)C6H3F2-2,5)]2 ∙ ½PhH ∙ ½C8H18 (1) and tri(para-tolyl)antimony bis(2-furancarboxylate) (4-MeC6H4)3Sb[OC(O)C4H4O]2 (2), obtained by oxidative addition reaction from triarylantimony and 2,5-difluorobenzoic/2-furancarboxylic acid in the presence of tertiary butyl hydroperoxide in ether, was established by X-ray diffraction analysis (XRD). According to the X-ray diffraction data, crystals 1 [C42H36Br3F4O7Sb, M 1090.19; triclinic system, symmetry group P-1; cell parameters: a = 12.899(11), b = 13.655(11), c = 14.558(14) Å; a = 100.48(5)°, β = 96.66(3)°, g = 116.57(3)°; V = 2197(3) Å3; Z = 2; rcal = 1.648 g/cm3; 2q: 6.092-49.572°; total reflections 38047; independent reflections 7448; number of specified parameters 546; Rint = 0.0464; GOOF 1.052; R1 = 0.0460, wR2 = 0.1218; residual electron density (max/min): 1.14/-1.07 e/Å3]; 2 [C31H27O6Sb, M 617.28; triclinic system, symmetry group P-1; cell parameters: a = 10.287(4), b = 11.776(6), c = 12.872(5) Å; a = 83.83(2)°, β = 83.694(16)°, g = 64.150(15)°; V = 1391,7(10) Å3, Z = 2; rcalc = 1.473 g/cm3; 2q: 5.62-77.32 degrees; total reflections 103088; independent reflections 15758; number of specified parameters 346; Rint = 0.0388; GOOF 1.020; R1 = 0.0409, wR2 = 0.0935; residual electron density (max/min): 1.12/-0.71 e/Å3] consist of trigonal bipyramidal molecules with electronegative ligands in axial positions. The Sb-C bond lengths vary in the range of 2.106(5)-2.112(5) Å for 1 and lower than in 2: 2.1108(18)-2.119(2) Å; the OSbO bond angles take values of 179.06(14)° and 177.07(4)°, respectively. The Sb-O distances in 1 (2.095(4) and 2.105(4) Å) are shorter than in 2 (2.1394(14) and 2.1566(14) Å). The Sb∙∙∙O intramolecular contacts between the central metal atom and carbonyl oxygen atom in 1 (3.113(6) and 3.130(6) Å) are significantly greater than in 2 (2.771(5) and 2.818(5) Å) and do not exceed the sum of ther van der Waals radii (3.7 Å). In addition, crystal 1 contains short contacts between the antimony atom and oxygen atom of the methoxy groups (3.067(6), 3.166(6), and 3.221(6) Å). Complete tables of atomic coordinates, bond lengths and bond angles for structures have been deposited in the Cambridge Structural Data Bank (No. 2060559 (1), No. 1979824 (2), deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).