A New Method for the Synthesis of Tetraphenylbismuth 1-Naphthalenesulfonate
The reaction of pentaphenylbismuth with triphenylantimony bis (1-naphthalenesulfonate) in benzene led to tetraphenylbismuth 1-naphthalenesulfonate, yielding 38%, which after recrystallization from water was identified as Ph<sub>4</sub>BiOSO<sub>2</sub>C<sub>10</sub>H<sub>7</sub> × H<sub>2</sub>O hydrate (1). Structure 1 (colorless crystals with mp 178 °C) was determined by X-ray diffraction analysis (XRD) on an automatic four-circle D8 Quest Bruker diffractometer (Мо К<sub>α</sub> radiation, λ = 0.71073 Å, graphite monochromator) at 293 K. Crystal size 0.27 × 0.25 × 0.09 mm, P- 1, a = 9.542 (5), b = 12.595 (5), c = 13.998 (5) Å, a = 74.228 (15), β = 80.06 (2), g= 68.758 (15) deg., V = 1503.7 (12) Å3, Z = 2. Data collection area for 2q equaled 5.72-77.8°, reflection index intervals were -16 ≤ h ≤ 16, -22 ≤ k ≤ 22, -24 ≤ l ≤ 24; a total of 102981 reflections were measured, 17181 independent reflections, refinement variables 364, μ = 5.968 mm<sup>-1</sup>; GOOF 0.987, the final values of the divergence factors R<sub>1</sub> = 0.0534 and wR <sub>2</sub> = 0.0941 (for reflexes F<sup>2</sup>> 2s (F<sup>2</sup>), R<sub>1</sub> = 0.1619 and wR <sub>2</sub> = 0.1163 (for all reflections), residual electron density 2.65 /-1.05 e/Å<sup>3</sup>. The bismuth atom in molecule 1 has a strongly distorted trigonal-bipyramidal coordination with the arenesulfonate substituent in the axial position. The СBiС bond angles are 100.52 (8) -119.28 (7)°, the Bi-C and Bi-O distances are 2.179 (2) -2.212 (2) and 2.915 (1) Å, respectively. Two molecules 1 are combined into dimers through hydrogen bonds between the hydrogen atoms of two water molecules and the oxygen atoms of two naphthalenesulfonate groups.