Synthesis and structure of tris(2-methoxyphenyl)antimony bis[3,4-difluorobenzoate] [(2-MeO)C6H4]3Sb[OC(O)C6H3(F2-3,4)]2 and tris(2-methoxyphenyl)antimony bis[benzenesulfonate] [(2-MeO)C6H4]3Sb[OSO2C6H5]2

Abstract

Tris(2-methoxyphenyl)antimony bis[3,4-difluorobenzoate] (1) and tris(2-methoxyphenyl)antimony bis[benzenesulfonate] (2) were obtained by oxidative addition reaction from triarylantimony and 3,4-difluorobenzoic/benzenesulfonic acid in the presence of tertiary bu-tyl hydroperoxide in ether. The structure of 1 and 2 was established with the use of IR spectrosco-py and X-ray diffraction analysis (XRD). Crystals 1 [C35H27O7F4Sb, M 757.32; triclinic syngony, symmetry group P–1; cell parameters: a = 9.219(4), b = 9.507(6), c = 20.240(11) Å; a = 99.43(3)°, β = 95.756(16)°, g = 107.90(3)°; V = 1643.6(16) Å3; Z = 2; rcalc = 1.530 g/cm3; 2q 6.68-54.98 de-grees; total reflections 31858; independent reflections 7153; number of specified parameters 427; Rint = 0.0429; GOOF 1.051; R1 = 0.0265, wR2 = 0.0551; residual electron density (max/min); 0.30/-0.44 e/Å3], 2 [C33H31O9S2Sb, M 757.46; monoclinic system, symmetry group C2/c; cell parame-ters: a = 21.157(9), b = 10.363(4), c = 18.285(7) Å; β = 126.590(13) deg., V = 3219(2) Å3, Z = 1; rcalk = 1.563 g/cm3; 2q 6.012-54.234 degrees; total reflections 32454; independent reflections 3541; number of specified parameters 231; Rint = 0.0283; GOOF 1.161; R1 = 0.0283, wR2 = 0.0659; residual electron density (max/min); 0.74/-0.83 e/Å3] consist of trigonal bipyramidal molecules with electronegative ligands in axial positions. The Sb–C bond lengths vary in the range 2.093(2)−2.125(3) Å, The OSbO bond angles take values 176.63(6)° and 174.52(10)°, respective-ly. The Sb–O distances in 1 (2.1106(17) and 2.1149(17) Å) are shorter than in 2 (2.128(2) and 2.128(2) Å). Intramolecular Sb∙∙∙O contacts in 1 (3.162(2) and 3.257(2) Å) are significantly smaller than in 2 (3.617(2) and 3.617(2) Å) and do not exceed the sum of their van der Waals radii (3.7 Å). Complete tables of atomic coordinates, bond lengths and bond angles for structures have been de-posited in the Cambridge Structural Data Bank (No. 2123247 (1), No. 2116583 (2), depos-it@ccdc.cam.ac.uk; http://www.ccdc cam.ac.uk).