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2O (1.333 g, 5 mmol) in distilled water (25 mL). The solution immediately became suspension and was stirred for 4 h at 60 oC. Then 4-mim (0.821 g, 10 mmol) ligand in methanol (10 mL) was added dropwise to this suspension. The clear solution was stirred for 2 h at 60 °C and then cooled to room temperature. The crystals formed were filtered and washed with 10 mL of water and were dried in air. Elemental Analysis; Calc. (%) : C, 40.50; H, 3.97; N, 20.99%; Exp. (%) : C, 40.85 ; H, 3.84 ; N, 21.06% .
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2O (1.333 g, 5 mmol) in distilled water (25 mL). The solution immediately became suspension and was stirred for 4 h at 60 oC. Then 4-mim (0.821 g, 10 mmol) ligand in methanol (10 mL) was added dropwise to this suspension. The clear solution was stirred for 2 h at 60 °C and then cooled to room temperature. The crystals formed were filtered and washed with 10 mL of water and were dried in air. Elemental Analysis; Calc. (%) : C, 40.50; H, 3.97; N, 20.99%; Exp. (%) : C, 40.85 ; H, 3.84 ; N, 21.06%.
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note
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-3, Rint = 0.043 and wR = 0.072 for 4500 independent reflections. A diffraction experiment was carried out at 293(2) K on a Stoe IPDS diffractometer. The structure was solved by direct methods and refined using the programs Shelxs97 and Shelxl97 [44]. All non-hydrogen atoms were refined anisotropically by full-matrix least-squares methods [44]. The H atom of the water was located in a difference map and later restrained to the distance O-H = 0.82 (2) Å. The other H atoms were positioned with idealized geometry using a riding model with C-H = 0.93-0.96 Å. Data collection: X-Area, cell refinement: X-Area, data reduction: X-RED [45]; program(s) have been used for molecular graphics: Mercury for Windows [46]; software has been used to prepare material for publication: WinGX [47].
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