Crystal structure of 3,4-dihydroxy-1,5-dimethyl-2-phenylpyrazolium chloride, [C11H13N2O2]Cl

Abstract

C 11 H 13 ClN 2 O 2 ,triclinic, P1 (no. 2), a =7.150(5) Å, b =8.380(2) Å, c =10.586(2) Å, a =71.80(2)°, b =84.05(5)°, g =87.47(5)°, V =599.3 Å 3 , Z =2, R gt(F) =0.049, wRref(F 2 ) =0.176, T =293 K. Source of materialThe title compound was obtained by dissolving 4-hydroxyantipyrine (0.408 g, 0.002 mole) in acetonitrile (10 ml) and then adding carefully of titanium tetrachloride (0.39 g, 0.002 mole) under nitrogen. Aw eek later white crystals appear from the acetonitrile solution. TiCl 4 catalyzes the reaction. As uitable crystal was taken for X-ray diffraction studies. Experimental detailsThe two Ha toms involved in hydrogen bonding (H1 and H2) were first located from adifference Fourier map and then refined isotropically. Other Hatoms were positioned geometrically and treated as riding on their parent atoms withThe attempts at recrystallization of the compound did not improve crystals quality, which explains the relatively large residual values.