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1,10-Phenanthroline was oxidized to 1,10-phenanthroline-5,6-dione according to the literature: Hiort, C. Lincoln, P. Norden, B. J. Am. Chem. Soc. 1993, 115, 3448. Preparation of HNCP·2.5H 2O: A mixture of 2 mmol 1,10-phenanthroline-5,6-dione, 2.2mmol 4-carboxybenzaldehyde, 15 mL of glacial acetic acid, and 3.2 g f ammonium acetate in a 100 mL flask with a condenser was refluxed for 2 h, resulting in a yellow precipitate. After cooling, the mixture was diluted with 25 mL of water and the pH value of the solution was adjusted with concentrated aqueous ammonia to 5.5. The yellow product was filtered from the mixture and washed with water and acetone, oven-dried at 60°C (yield: 87% based on 1,10-phenanthroline-5, 6-dione, Mp: 305-307°C Anal. Caled for HNCP·2.5H2O: C, 62.33; H, 4.45; N, 14.54; O, 18.68. Found: C, 62.41; H, 4.38; N, 14.58; O, 18.61. 1H NMR DMSO, 9.05 d 2H, 8.96 d 2H, 8.42 d 2H, 8.19 d 2H, 7.85 dd
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Preparation of [Mn(NCP)2Jn(1, hydrothermal treatment of MnSO4 (0.3 mmol, HNCP·2.5H2O (0.5 mmol) and H2O (25 mL) in an autoclave at 180°C for 3 days gave orange crystals of 1 (yield: 85% based on HNCP, Anal. Caled for Mn 1C40H22N8O4: C, 65.49; H, 3.02; N, 15.27; O, 8.72. Found: C, 65.43; H, 3.06; N, 15.21; O, 8.78. IR (KBr pellet, cm-1, 3435br, 1597s, 1535m, 1475w, 1449w, 1389s, 1274w, 1069m, 948w, 877w, 838w, 806m, 776m, 731m, 717m. Crystal data for compound 1: fw 733.60, orthorhombic, Aba2, a, 15.4071(12) Å, b= 20.450(2) Å, c, 9.9044(10) Å, V, 3120.6(5, Z, 4, ρcalcd, 1.561 g cm-3, p, 0.485 mm-1, R1/wR2, 0.0467/0.1106 (1 > 2σ) and 0.0598/0.1189 (all data, Flack parameter value, 0.043
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