Journal of the Korean Chemical Society (대한화학회지)

Korean Chemical Society (대한화학회)
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Synthesis and Crystal Structures of Copper(II) Complexes with Schiff Base Ligands

  • Koo, Bon Kweon (Department of Life Chemistry, Catholic University of Daegu)
  • Received : 2014.11.10
  • Accepted : 2014.12.17
  • Published : 2015.02.20
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Abstract

Keywords

EXPERIMENTAL

Chemicals and Measurements

All chemicals are commercially available and were used as received without further purification. The ligands, Hapb and Hbpb were prepared as described in the literature.28,29 Elemental analyses (CHN) were performed on a Vario EL EA-Elementar Analyzer.

Preparation of [Cu2(apb)2(HBA)(ClO4)]·0.5H2O (1)

To a methanolic solution (20 mL) of Hapb (0.239 g, 1 mmol) was added Cu(ClO4)2·6H2O (0.371 g, 1 mmol). To the result ing solution was added a methanolic solution (3 mL) of H2 BA (0.228 g, 1 mmol) and triethylamine (0.101 g, 1 mmol). The solution turned to green and was refluxed for 3 h to yield green solid. The solid was isolated by filtration and airdried. The yellow filtrate was kept at room temperature to give green block crystals in good quality for X-ray crystallography. Yield: 63% (0.296 g) based on Cu. Anal. Calcd. for C42H36N6O9.5ClCu2: C, 53.70; H, 3.86; N, 8.95. Found: C, 53.83; H, 3.92; N,8.92%.

Preparation of [Cu(bpb)2] (2)

The compound was prepared similarly by the method described above for the preparation of 1, with use of Hbpb instead of Hapb ligand. The green solid was recrystallized from the CH3OH/(C2H5)2O= 1:2 solution to give black block crystals in good quality for X-ray crystallography. Yield: 72% (0.480 g) based on Cu. Anal. Calcd. For C38H28N6O2Cu: C, 68.72; H, 4.25; N, 12.65. Found: C, 68.45; H, 4.41; N,12.30%.

X-ray Structure Determination

Single crystals of 1 and 2 were obtained by the method described in the above procedure. Structural measurement for the complexes were performed on a Bruker SMART APEX CCD diffractometer using graphite monochromatized Mo-Kα radiation (λ = 0.71073 Å) at the Korea Basic Science Institute. The structure was solved by direct method and refined on F2 by full-matrix least-squares procedures using the SHELXTL programs.30 All non-hydrogen atoms were refined using anisotropic thermal parameters. The hydrogen atoms were included in the structure factor calculation at idealized positions by using a riding model, but not refined. Images were created with the DIAMOND program. 31

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