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2O (0.1542 g, 0.5 mmol) for 2, oxalic acid (0.0189 g, 0.15 mmol) and 4,4-bipyridine (0.0288 g, 0.15 mmol) were dissolved in 3 ml of ethylene alcohol and 5 ml of distilled water upon oscillating in the ultrasonic oscillator for 30 min. The mixture was then sealed in a 15 ml Teflon-lined autoclave, and kept in the oven at 120 °C for 7 days. After the autoclave was cooled at room temperature, red rhombic crystals were filtered off, washed with distilled water, and dried in a desiccator at room temperature. Yield: 30.5% for 1, and 28.2% for 2 (based on Co).
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-1, F(0 0 0) = 307. Final residuals with R1 = 0.0354 and wR2 = 0.1220 with [I > 2 δ(I)], and R1 = 0.0360 and wR2 = 0.0978 for all data. The single-crystal X-ray data was collected on a Bruker SMART CCD diffractometer with graphite-monochromated Mo Kα radiation (λ = 0.71073 Å) at room temperature. Data reductions and absorption corrections were performed using the SAINT and SADABS software packages, respectively. The structure was solved by direct methods and refined by full matrix least-squares methods on F2 using the SHELXS-97 and SHELXL-97 programs, using atomic scattering factors for neutral atoms. Anisotropic displacement parameters were refined for all non-hydrogen atoms. The hydrogen atoms were located from difference Fourier maps.
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