A new two dimensional copper (II) coordination complex with sulphonamide: Synthesis, crystal structure and DNA binding study

Author:

Devi W. Bembee,Singh R.K. Bhubon,Jasinski J.P.,Golen J.A.

Funder

UGC

NSF-MRI

Publisher

Elsevier BV

Subject

Materials Chemistry,Inorganic Chemistry,Physical and Theoretical Chemistry

Reference19 articles.

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3. Synthesis and biological evaluation of Schiff base of dapsone and their derivative as antimicrobial agents;Wadher;Int. J. Pharm. Tech Res.,2009

4. Toward efficient Zn(II)-based artificial nucleases;Boseggia;J. Am. Chem. Soc.,2004

5. All the reagents were of analytical reagent grade. (A) The Sulphonamide imine Schiff base ligand was prepared by refluxing sulphanilamide (2 mmol, 0.328 g) and Benzoylacetone (2 mmol, 0.326 g) in about 15 ml of methanol for 3 hours at ca. 70⁰C in presence of 1–2 drops of conc. H2SO4. The precipitated light yellow coloured ligand was filtered and air dried. The purity of the ligand was checked by TLC and melting point determination method. Yield: 2.74 g (~90%). M.P.: 154⁰C. Anal. Calc. for C16H16N2O3S (M.W.: 316.04 g/mol): C, 60.50; H, 4.73; N, 4.42. Found: C, 60.49; H, 4.68; N, 4.33. (B) The title copper(II) complex was synthesized by reaction of the above prepared ligand (2 mmol, 0.638 g) with copper acetate monohydrate (1mmol, 0.198 g) in about 20 ml of methanol solution at 70⁰C. Block, black coloured single crystals suitable for X-ray analysis was obtained on slow evaporation of the reaction mixture solution. Yield: 0.55 g (~80%). Anal. Calc. for C32H30 CuN4O6S2 (M.W.: 694.26 g/mol): C, 55.31; H, 4.32; N, 8.07. Found: C, 55.21; H, 4.36; N, 8.17. μeff=1.78 B.M. The diffraction data of a block, black crystal (size 0.22x 0.15x 0.12 mm) was collected on an Oxford Diffraction Gemini-E CCD system with graphite monochromated MoKα (λ=0.71073) at 170 K. Data reduction and an absorption correction were performed with the CrysAlis program [18]. The structure of the complex was solved by direct methods using the SHELX97 software [19]. The non-H-atoms were anisotropically refined using the full-matrix least square method on F2. Hydrogen atoms H3A, H3B, H4A, and H4B were allowed to refine at N---H distance restraints of 0.87(1) Å and H---N---H angle restraints of 1.35(2) Å. All remaining hydrogen atoms were placed at calculated positions and refined riding on the parent atoms with atom-hydrogen lengths and isotropc displacement parameters (CH) 0.95 Å and ~1.2 times Ueq of the parent atoms, (CH3) 0.98 Å and ~1.5 times Ueq of the parent atoms. Refinement of the C5 thermal amplitude was adjusted with an ISOR constraint. Crystal data: C32 H30 Cu N4 O6 S2, Mr. 694.26 g mol-1, Orthorhombic space group Pca2 (1), a=19.9292(11) Å, b=5.4243(4) Å, c=28.6159(18) Å, V=3093.4 93) Å-3, Z=4, Dc=1.491 Mg m-3, F(000)=1436, R1=0.0757, wR2=0.1333

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