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72249122662
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A mixture of water solution (10 mL) of 1,2-bis(4-pyridyl)ethylene (0.180 g, 1.0 mmol) and 5-nitro-isophthalic acid (0.211 g, 1.0 mmol) was added Co(NO3)2·6H2O (0.292 g, 1.0 mmol) and 0.75 mL triethylamine dropwisely to a stirring aqueous solution (5 mL) for 10 min at room temperature. The reactants were sealed in a 23-mL Teflon-lined autoclave heated at 140 °C for 4 days. Then red block crystals were obtained. The crystals were picked out, washed with distilled water and dried in air (Yield. ca. 62, based on Co, Calcd, ) for C56H36Co4N8O26: C, 45.67; H, 2.46; N, 7.61. Found C, 45.72; H, 2.53; N, 7.58. IR data (KBr, cm-1, 3428 (s, 3067 (w, 1602 (s, 1578 (s) 1552 (m, 1389 (s, 1112 (m, 827 (m, 778 (m, 636 (m, 475 w, Fig. S2
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-1): 3428 (s), 3067 (w), 1602 (s), 1578 (s) 1552 (m), 1389 (s), 1112 (m), 827 (m), 778 (m), 636 (m), 475 (w) (Fig. S2).
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72249089658
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Crystal data for 1: C56H36Co4N8O26, Mr, 1472.65, Triclinic, space group P over(1, ̄, a, 11.811(6) Å, b, 15.579 (8) Å, c, 15.875(8) Å, V, 2794.3(2) Å3, α, 92.089(1)o, β, 101.273(1)o, γ, 101.883(1)o, Z, 2, Dcalcd, 1.750 g/cm3, μ, 1.267 mm-1, R1[I>2σ(I, 0.0328, wR2for all data, 0.0902. The structure was solved by direct methods and refined by full-matrix least-squares fitting on F2 by SHELXL-97
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2 by SHELXL-97.
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