Synthesis and structure of triphenylbismuth bis(2,4-dimethylbenzenesulphonate) hydrate

The interaction of triphenylbismuth with 2,4-dimethylbenzenesulfonic acid in diethyl ether in the presence of tert-butyl hydroperoxide have synthesized triphenylbismuth bis(2,4-dimethylbenzenesulfonate) hydrate. The X-ray diffraction pattern has been obtained at 293 K on an automatic diffractometer D8 Quest Bruker (MoKα-radiation, λ = 0.71073 Å, graphite monochromator) of crystals 1 [C34H34O6,5S2Bi, M 819.71, monoclinic syngony, symmetry group C2/c; cell parameters: a = 34.948(16) Å, b = 9.210(5) Å, c = 21.114(9) Å, α = γ = 90.00 degrees, β = 99.97(2) degrees; V = 6693(6) Å3; the crystal size is 0.38 × 0.14 × 0.06 mm; intervals of reflection indexes are -45 ≤ h ≤ 45, -11 ≤ k ≤ 11, -27 ≤ l ≤ 27; total reflections 52257; independent reflections 7691; GOOF 1.026; R1 = 0.0325, wR2 = 0.0776; residual electron density is 0.98/-0.82 e/Å3] the bismuth atom have a distorted trigonal-bipyramidal coordination. The OBiO axial angles are 171.58(12) degrees; the sum of the CBiC angles in the equatorial plane is 360 degrees. The lengths of the Bi-O axial bonds are 2.274(3) Å and 2.284(3) Å; The range of changes in the lengths of the Bi-C equatorial bonds is 2.188(5)-2.209(4) Å. The structure of triphenylbismuth bis(2,4-dimethylbenzenesulfonate) hydrate contains intramolecular contacts between the bismuth and oxygen atoms of the sulfonate ligands; the Bi···O=S distances are 3.178(10) and 3.261(10) Å, which is less than the sum of the Van der Waals radii of bismuth and oxygen (3.59 Å). A water molecule is connected by a hydrogen bond O-H···O=S 2.50 Å with the oxygen atom of the sulfonate ligands. Complete tables of atomic coordinates, bond lengths, and bond angles for the structures were deposited at the Cambridge Crystallographic Data Center (no. 1919942, deposit@ccdc.cam.ac.uk, http://www.ccdc.cam.ac.uk).