4-nitrophenylacetates of tetra- and tri-(para-tolyl) antimony. Synthesis and structural features

The interaction of penta( para -tolyl)antimony with 4-nitrophenylacetic acid in toluene have synthesized tetra( para -tolyl)antimony 4-nitrophenylacetate (1). The reaction of tri( para -tolyl)antimony with tert -butyl hydroperoxide and 4-nitrophenylacetic acid in diethyl ether leads to the formation of tri( para -tolyl)antimony bis (4-nitrophenylacetate) (1). 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) of crystals 1 [C72H68N2O8Sb2, M 1332.78, the triclinic syngony, the symmetry group P -1; cell parameters: a 12.08(3), b 16.46(3), c 17.79(3) Å, α = 107.61(7) degrees, β = 97.20(10) degrees, γ = 101.94(9) degrees; V = 3229(11) Å3; the crystal size is 0.51×0.24×0.17 mm; intervals of reflection indexes are -10 ≤ h ≤ 10, -14 ≤ k ≤ 14, -15 ≤ l ≤ 15; total reflections 14622; independent reflections 4546; Rint 0.0697; GOOF 1.072; R 1 = 0.0585, wR 2 = 0.1688; residual electron density 0.75/-0.85 e/Å3] and 2 [C37H33O8N2Sb, M 755.40, the monoclinic syngony, the symmetry group P2 1 /n ; cell parameters: a 9.271(2), b 28.413(7), c 13.604(3) Å, α = 90.00 degrees, β = 105.876(2) degrees, γ = 90.00 degrees; V = 3425.5(13) Å3; the crystal size is 0.95×0.58×0.34 mm; intervals of reflection indexes are -16 ≤ h ≤ 16, -50 ≤ k ≤ 50, -24 ≤ l ≤ 24; total reflections 125931; independent reflections 20517; Rint 0.0450; GOOF 1.114; R 1 = 0.0511, wR 2 = 0.0993; residual electron density 0.70/-0.97 e/Å3] the antimony atoms have distorted trigonal-bipyramidal coordination. The axial angles of OSbC and OSbO are 177.9 (5)°, 177.9 (5)° (1) and 177.27(5)° (2); the sum of the angles of CSbC in the equatorial plane is 356.9°, 357.6° (1), 359.79° (2). The Sb-O and Sb-C bond lengths are 2.1443(15)-2.269(10) Å and 2.098(15)-2.170(14) Å. The structural organization of crystals 1 and 2 is controlled by intermolecular bonds O···H (2.46-2.67 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. 1819287, 1819295; deposit@ccdc.cam.ac.uk; http: //www.ccdc. Cam.ac.uk).