Synthesis and Structure of Tetraphenylantimony 1-Naphtalenesulfonate

Abstract

Interaction of equimolar amounts of pentaphenylantimony and 1-naphtalenesulfonic acid in benzene led to tetraphenylantimony 1-naphtalene monohydrate Ph₄SbOSO₂Naft-1∙H₂O (1), the structure of which was then characterized. According to the X-ray diffraction data, obtained on an automatic four-circle D8 Quest Bruker diffractometer (two-axis CCD detector, МоК_α radiation, λ = 0.71073 Å, graphite monochromator) at 293 K for crystal 1: [C₃₄H₂₉O₄SSb, M 655.38; triclinic syngony, symmetry group Р-1; cell parameters: a = 9.456(3), b = 12.541(4), c = 13.980(6) Å; α = 74.151(15) deg., β = 79.979(19) deg., γ = 68.178(12) deg.; V = 1475.7(9) ų; crystal size 0.5×0.5×0.23 mm; reflection index intervals –12 ≤ h ≤ 12, –16 ≤ k ≤ 16,
–18 ≤ l ≤ 18; total reflections 20654; independent reflections 5934; R_int 0.0385; GOOF 1.202;
R₁ = 0.1215, wR₂ = 0.3556; residual electron density 1.98/-2.53 e/ų], the antimony atoms have a distorted trigonal-bipyramidal coordination with the carbon and oxygen atoms in the axial positions (the CSbO angle is 172.3(6)°, the Sb∙∙∙O distance equals 2.84(1) Å). The Sb-C and S-O bond lengths in 1 change within a narrow range (2.000(13)-2.132(13) Å and 1.441(4)-1.456(4) Å). The structural organization in crystal 1 is caused by weak intermolecular contacts of the S=О···Н–C type, 2.50–2.71 Å. Complete tables of atom coordinates, bond lengths and valence angles for structure 1 are deposited at the Cambridge Crystallographic Data Center (No. 2115624; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).