Synthesis and crystal structure of 3-ammonium-4-hydroxyphenyl sulfonate hemihydrate
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TRUCTURE OF ORGANIC COMPOUNDS
Synthesis and Crystal Structure of 3Ammonium4Hydroxyphenyl Sulfonate Hemihydrate1 M. Belhouchet and T. Mhiri Solid State Laboratory, Sfax Faculty of Science, University of Sfax, BP 1171, 3000 Sfax, Tunisia email: [email protected] Received September 29, 2011
Abstract—The crystal structure of 3ammonium4hydroxyphenyl sulfonate hemihydrate C6H3(NH3)(OH)SO3 · 0.5H2O is determined by singlecrystal Xray diffraction. The unit cell parameters are as follows: a = 11.2395(3), b = 10.3814(3), c = 13.7509(4) Å, β = 100.326(1)°, V = 1578.49(8) Å3, space group P21/n, Z = 4. The crystal structure can be described us a succession of infinite corrugated layers parallel to ab plane. These layers consist of rings formed by four sulfonate molecules located around a center of sym metry. The rings are connected to each other and to water molecules via O–H···O hydrogen bonds. The struc ture is further stabilized by π–π interactions between phenyl rings of organic entities of successive layers. DOI: 10.1134/S106377451301015X 1
INTRODUCTION
Weak interactions, such as hydrogen bonding and π–π stacking, have attracted much interest owing to their significance in chemistry and biology, especially in the field of crystal engineering [1, 2]. The amine and sulfonate moieties are important constituents of many important compounds developing welldefined noncovalent supramolecular architectures because of their ability to form multiple hydrogen bonds. As a part of studying the hydrogen bonding patterns of this class of compounds, in the present work, the crystal structure of 3ammonio4hydroxyphenyl sulfonate hemihydrate (I) has been determined by Xray dif fraction.
Table 1. Crystal data and structure refinement parameters of C6H3(NH3)(OH)SO3 ⋅ 0.5H2O
EXPERIMENTAL Synthesis. The title compound was obtained by dissolving 0.3 g 3amino4hydroxyphenyl sulfam inic acid in a dilute HCl (37%). Pink single crystals suitable for Xray diffraction appear after some days in the course of slow evaporation of the obtained solution at room temperature. These crystals are stable, for long time, in normal conditions of tem perature and humidity. Crystal structure determination. A block single crys tal of the title compound was selected for the Xray structure analysis. Unit cell parameters were deter mined by least squares on the basis of 8518 reflections. The structure was solved with direct method, from the SHELXS97 program [3], which permitted the loca 1 The article is published in the original.
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System, sp. gr., Z a, b, c, Å V, Å3 Dx, g cm–3 Radiation, λ, Å μ, mm–1 T, K Sample size, mm Diffractometer Scan mode Absorption correction, Tmin, Tmax θmax, deg h, k, l ranges Number of reflections: measured/unique (N1), Rint /with I > 2σ(I) (N2) Refinement method Number of refined parame ters Reliability factors: wR2 relative to N1 R1 relative to N2 S Δρmax/Δρmin, e/Å3 Program package
Monoclinic, P21/n, 4 11.2395(3), 10.3814(3), 13.7509(4) 1578.49(8) 1.312 MoKα, 0.71073 1.668 293 (2) 0.32 × 0.25 × 0
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