Reaction of tetraphenylantimony acetylacetonate with mesitylenesulfonic acid

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; rcalc = 1.435 g/cm3; m = 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; a = 90.00°, β = 90.00°, g = 90.00°, V = 2446(5) Å3, Z = 8; rcalc = 1.278 g/cm3; m = 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).