Reaction of tetraphenylantimony acetylacetonate with mesitylenesulfonic acid

Abstract

Tetraphenylantimony mesitylenesulfonate (1) is formed with a yield of 78% from mesitylenesulfonic acid (2) and tetraphenylantimony acetylacetonate in an aqueous-acetone solution. According to X-ray diffraction analysis, the antimony atoms in complex 1 have the coordination of a distorted trigonal bipyramid with an axially located mesitylenesulfonate ligand, while the CSbO axial angle is 173.99(5), and the SbO distance is 2s4717(15) Å. Crystal 2 consists of molecules of hydration water and mesitylenesulfonic acid. Crystallographic characteristics 1 [C33H31O3SSb, M = 629.39; monoclinic system, sp. gr. P21/n; cell parameters: a = 10.098(5) Å, b = 14.125(6) Å, c = 20.777(11) Å; β = 100.59(2), V = 2913(2) Å3, Z = 4; calc = 1.435 g/cm3;  = 1.050 mm–1; F(000) = 1280.0; collection at 2q: 5.92–55.02; –13 ≤ h ≤ 13, –18 ≤ k ≤ 18, –26 ≤ l ≤ 26; total reflections 80722; independent reflections 6675 (Rint = 0.0313); GOOF = 1.078; R-factor = 0.0222]; 2 [C9H15O5S, M = 235.27; rhombic system, sp. gr. Pbca; cell parameters: a = 15.221(17) Å, b = 7.882(8) Å, c = 20.39(3) Å;  = 90.00, β = 90.00,  = 90.00, V = 2446(5) Å3, Z = 8; calc = 1.278 g/cm3;  = 0.264 mm–1; F(000) = 1000.0; collection at 2q: 6.16–54.46; –19 ≤ h ≤ 19, –9 ≤ k ≤ 9, –26 ≤ l ≤ 26; total reflections 32479; independent reflections 2628 (Rint = 0.0768); GOOF = 1.025; R-factor = 0.0650]. Complete tables of atomic coordinates, bond lengths and bond angles of compounds 1 and 2 have been deposited in the Cambridge Structural Data Center (CCDC 2335253 and 2332598; deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).