Synthesis and structure of the acetone solvate of tetra(para-tolyl)antimony 2,4-dinitrobenzensulfonate

By the interaction of equimolar amounts of penta-para-tolylantimony with 2,4-dinitrobenzenesulfonic acid in benzene, followed by recrystallization from aqueous acetone, the tetra-(para-tolyl)antimony 2,4-dinitrobenzenesulfonate acetone solvate Tol4SbOSO2C6H3(NO2)2-2.4 ∙ Me2C=O (1) was obtained and structurally characterized. According to X-ray diffraction analysis of crystal 1 [C37H37N2O8SSb, M 791.50; monoclinic syngony, space group C2/c; cell parameters: a = 23.232(13), b = 13.522(9), c = 23.812(15) Å; β = 102.22(3) degrees.; V = 7311(8) Å3; crystal size 0.4 × 0.14 × 0.07 mm; reflection index intervals -34 ≤ h ≤ 34, -19 ≤ k ≤ 19, -35 ≤ l ≤ 31; total reflections 111477; independent reflections 12261; Rint 0.0870; GOOF 1.009; R1 = 0.0411, wR2 = 0.0710; residual electron density 0.37/-0.68 e/Å3] performed by an automatic four-circle D8 Quest Bruker diffractometer (MoKα radiation, λ = 0.71073 Å, graphite monochromator) at 293 K, the antimony atoms have a distorted tetrahedral coordination (the СSbС angles are 99.85(9)°- 123.74(9)°). However, due to the coordination of one of the sulfo group oxygen atoms with the central metal atom (the Sb∙∙∙O distance is 2.814(4) Å) it is more correct to consider the coordination of the central metal atom as trigonal-bipyramidal (axial angle O(1)Sb(1)C(11) 172.78(8)°, the equatorial angles are 123.74(8), 114.60(8), 102.92(8)°). The Sb-C bond lengths in compound 1 vary in a narrow interval (2.091(2)-2.111(2) Å). The structural organization in crystal 1 is caused by weak intermolecular contacts of the О···Н-C type, 2.25-2.69 Å. Complete tables of coordinates of atoms, bond lengths and valence angles for structure 1 are deposited at the Cambridge Structural Data Bank (No. 2123785; deposit@ccdc.cam.ac.uk; http: //www.ccdc.cam.ac.uk).