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Synthesis of 1 ⊃ solvent: A solid mixture of H3BTB 1 mg, 0.025 mmoland Cd(NO3)2·4H2O .7 mg, 0.025 mmolwas dissolved in a mixture of DMF/MeOH (0.5/0. 5 mLin an 2 mL glass vial. To this reaction mixture, a few drops of concd HNO3 was added and the initial pH = 2.0. The whole reaction mixture was heated in a temperature controllable oven from room temperature to 100 °C, over a period of 4 h and then at 100 °C for 48 h. The oven was cooled from 100 to 30 °C over a period of 6 h. The product contains homogeneous colorless flake-type crystals, which were isolated by washing with MeOH and dried in air. Yield: 15.8 mg, 80% based on 1 mol of H3BTB. Elemental microanalysis for [Cd2(HBTB)2(DMF) (MeOH)]·(DMF)4(MeOH)(DMA≡ C73H82N6O19Cd2, calcd (%): C, 55.76; H, 5.26; N, 5.35. Found (%): C, 56.95; H, 5.43; N, 5.21. FTIR 000-525 cm-1): 3417 (br, w), 3015
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Synthesis of 1 ⊃ solvent: A solid mixture of H3BTB 1 mg, 0.025 mmoland Cd(NO3)2·4H2O .7 mg, 0.025 mmolwas dissolved in a mixture of DMF/MeOH (0.5/0. 5 mLin an 2 mL glass vial. To this reaction mixture, a few drops of concd HNO3 was added and the initial pH = 2.0. The whole reaction mixture was heated in a temperature controllable oven from room temperature to 100 °C, over a period of 4 h and then at 100 °C for 48 h. The oven was cooled from 100 to 30 °C over a period of 6 h. The product contains homogeneous colorless flake-type crystals, which were isolated by washing with MeOH and dried in air. Yield: 15.8 mg, 80% based on 1 mol of H3BTB. Elemental microanalysis for [Cd2(HBTB)2(DMF) (MeOH)]·(DMF)4(MeOH)(DMA≡ C73H82N6O19Cd2, calcd (%): C, 55.76; H, 5.26; N, 5.35. Found (%): C, 56.95; H, 5.43; N, 5.21. FTIR 000-525 cm-1): 3417 (br, w), 3015 (s, w), 2760 (s, w), 1655(m), 1641 (s), 1577 (vs), 1523 (s), 1419 (w), 1370 (vs), 1243. ), 1178 (m), 1094 (m), 1013 (m), 852 (s), 793 (m), 782 (vs), 705. ), 668 (vs).
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35
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84876921975
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Synthesis of 2 ⊃ solvent: A solid mixture of H3BTB 1 mg, 0.025 mmoland Cd(NO3)2·4H2O .7 mg, 0.025 mmolwas dissolved in a mixture of DMF/MeOH/H2O (0.5/0.25/0.25 mLin an 2 mL glass vial. To the reaction mixture, 20 μL of NaOH (0.01 Mwas added as a deprotonating agent and the initial pH = 6.0. The whole reaction mixture was heated in a temperature controllable oven from room temperature to 100 °C, over a period of 4 h and then at 100 °C for 48 h. The oven was cooled from 100 to 30 °C over a period of 6 h. The product contains homogeneous colorless flake-type crystals, which were isolated by washing with MeOH and dried in air. Yield: 16 mg, 83% based on 1 mol of H3BTB. Elemental microanalysis for [Cd(HBTB)(DMF)]·(DMF)2 ≡ C36H37N3O9Cd, calcd (%): C, 56.29; H, 4.86; N, 5.47. Found (%): C, 56.13; H, 4.95; N, 5.24. FT-IR 000-525 cm-1): 3402 (br, w)
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Synthesis of 2 ⊃ solvent: A solid mixture of H3BTB 1 mg, 0.025 mmoland Cd(NO3)2·4H2O .7 mg, 0.025 mmolwas dissolved in a mixture of DMF/MeOH/H2O (0.5/0.25/0.25 mLin an 2 mL glass vial. To the reaction mixture, 20 μL of NaOH (0.01 Mwas added as a deprotonating agent and the initial pH = 6.0. The whole reaction mixture was heated in a temperature controllable oven from room temperature to 100 °C, over a period of 4 h and then at 100 °C for 48 h. The oven was cooled from 100 to 30 °C over a period of 6 h. The product contains homogeneous colorless flake-type crystals, which were isolated by washing with MeOH and dried in air. Yield: 16 mg, 83% based on 1 mol of H3BTB. Elemental microanalysis for [Cd(HBTB)(DMF)]·(DMF)2 ≡ C36H37N3O9Cd, calcd (%): C, 56.29; H, 4.86; N, 5.47. Found (%): C, 56.13; H, 4.95; N, 5.24. FT-IR 000-525 cm-1): 3402 (br, w), 3020 (s, w), 2777 (s, w), 1656(m), 1641 (s), 1576 (vs), 1526 (s), 1467 (w), 1416 (w), 1368 (vs), 1246. ), 1179 (m), 1095 (m), 1013 (m), 1011 (m), 874 (w), 853 (s), 811. ), 782 (v), 705 (m), 668 (s).
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84876900883
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Single crystal X-ray data for 1 ⊃ solvent: C73H82N6O19Cd2, fw = 1572.25, monoclinic, P21/n, a = 17.357), b = 26.425), c = 17.82Å, β = 116.889)°, V = 729Å3, Z = 4, ρcalc = 1.433. gcm-3, μ = 0.658 mm-1, GOF = 1.055, R1 = 0.0794, and wR2 = 0.2188. for 9788 reflections with I > 2σ(I
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Single crystal X-ray data for 1 ⊃ solvent: C73H82N6O19Cd2, fw = 1572.25, monoclinic, P21/n, a = 17.357), b = 26.425), c = 17.82Å, β = 116.889)°, V = 729Å3, Z = 4, ρcalc = 1.433. gcm-3, μ = 0.658 mm-1, GOF = 1.055, R1 = 0.0794, and wR2 = 0.2188. for 9788 reflections with I > 2σ(I).
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Single crystal X-ray data for 2 ⊃ solvent: C36H37N3O9Cd, fw = 768.09, monoclinic, P21/n, a = 14.915), b = 8.986), c = 26.75Å, β = 96.272)°, V = 356Å3, Z = 4, ρcalc = 1.431 gcm-3, μ = 0.670 mm-1, GOF = 1.103, R1 = 0.0609, and wR2 = 0.1530 for 8466. of reflections with I > 2σ(I
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Single crystal X-ray data for 2 ⊃ solvent: C36H37N3O9Cd, fw = 768.09, monoclinic, P21/n, a = 14.915), b = 8.986), c = 26.75Å, β = 96.272)°, V = 356Å3, Z = 4, ρcalc = 1.431 gcm-3, μ = 0.670 mm-1, GOF = 1.103, R1 = 0.0609, and wR2 = 0.1530 for 8466. of reflections with I > 2σ(I).
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