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 Ph4BiOSO2C10H7 × H2O 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 Кα 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-1; GOOF 0.987, the final values of the divergence factors R1 = 0.0534 and wR 2 = 0.0941 (for reflexes F2> 2s (F2), R1 = 0.1619 and wR 2 = 0.1163 (for all reflections), residual electron density 2.65 /-1.05 e/Å3. 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.