A New Method for the Synthesis of Tetraphenylbismuth 1-Naphthalenesulfonate

Abstract

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 (МоК_α 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 wR₂ = 0.0941 (for reflexes F²> 2s (F²), R₁ = 0.1619 and wR₂ = 0.1163 (for all reflections), residual electron density 2.65 /–1.05 e/ų. 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.