Crystal and molecular structure of adduct of 6-benzylaminopurine and 5-sulfosalicylic acid
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TRUCTURE OF ORGANIC COMPOUNDS
Crystal and Molecular Structure of Adduct of 6Benzylaminopurine and 5Sulfosalicylic Acid1 Min Xia and KuiRong Ma Jiangsu Key Laboratory for Chemistry of LowDimensional Materials, School of Chemistry and Chemical Engineering, Huaiyin Normal University, Huai’an, Jiangsu 223300, P.R. China email: [email protected] Received December 10, 2009
Abstract—The crystal structure of adduct of 6benzylaminopurine and 5sulfosalicylic acid C19H25N5O10S 1 is studied using singlecrystal diffraction (R = 0.0482 for 2852 reflections with I > 2σ(I)). The asymmetric unit of 1 contains one 6benzylaminopurine molecule and one 5sulfosalicylic acid molecule, as well as four lat tice water molecules. Hydrogen bonds, formed by 6benzylaminopurine and 5sulfosalicylic acid, link the two molecules into onedimensional chain (omitting four water molecules), further joined to twodimen sional layer network. Short ringinteractions with intrachain π–π stacking are observed. The data of IR spec troscopy confirm the formation of the twodimensional supramolecular layer structure. At last, a 3D supramolecular network constructs via hydrogen bonds. DOI: 10.1134/S1063774510070163 1 SAMPLE PREPARATION AND EXPERIMENTAL TECHNIQUE Synthesis The compound C19H25N5O10S 1 was synthesized using solvent volatile diffusion method by the reaction of 6benzylaminopurine 0.02 g (0.1 mmol) and 5sul fosalicylic acid 0.05 g (0.2 mmol) in deionized water 10 ml. The mixture (molar ratio 1 : 2) was sealed in a 15 ml Teflonlined stainless steel autoclave, and then heated at 120°C for 48 h. The crystals of 1 (yellow club shaped) was collected by vacuum filtration, washed thoroughly with deionized water and dried in air (yield 68%). IR absorption spectra of 1 were measured on an AVATA360 infrared spectrometer as KBr pellet in the 400–4000 cm–1 region. Xray diffraction analysis. Crystals 1, C19H25N5O10S (M = 515.51) are triclinic, a = 7.8884(13) Å, b = 10.6735(17) Å, c = 14.198(2) Å, α = 78.258(2)°, β = 80.286(3)°, γ = 88.593(18)°, V = 1153.6(3) Å3, Dx = 1.484 g/cm3, μ (MoKα) = 0.206 mm–1,
orangered clubbed crystal 0.28 × 0.20 × 0.15 mm in size. The reflections were collected in the index ranges –9 ≤ h ≤ 9, –12 ≤ k ≤ 12, –17 ≤ l ≤ 17. The structure was solved by direct methods (SHELXS97 [1]) and refined by the least squares pro cedure on F 2 (SHELXL97 [2]) in the fullmatrix anisotropic approximation for all nonhydrogen atoms. All hydrogen atoms were added according as theoretical models and refined in the isotropic approximation. The final discrepancy factors are as follows: R1 = 0.0482, wR2 = 0.1009, and S = 1.006 for 2852 reflections with I > 2σ(I). R1 = 0.0805 and wR2 = 0.1125 for all reflections. The total number of refined parameters is 316; and the residual (minimum and maximum) electron densities Δρmax and Δρmin are 0.308 and –0.432 eÅ–3, respectively. The bond dis tances and angles are listed in Table 1. The structure of 1 has been deposited with the Cambridge Structural Database (CCDC deposition no. 745590).
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