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Volumn 13, Issue 3, 2013, Pages 981-985

PH-dependent interpenetrated, polymorphic, Cd2+- and btb-based porous coordination polymers with open metal sites

Author keywords

[No Author keywords available]

Indexed keywords

2D STRUCTURES; 3D STRUCTURE; DIFFUSE REFLECTANCE; NET TOPOLOGY; POLYMORPHIC FORMS; POLYMORPHIC PHASIS; POROUS COORDINATION POLYMER; STRONG INTERACTION;

EID: 84876945373     PISSN: 15287483     EISSN: 15287505     Source Type: Journal    
DOI: 10.1021/cg301476p     Document Type: Article
Times cited : (70)

References (47)
  • 34
    • 84876937136 scopus 로고    scopus 로고
    • 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
    • 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).
  • 35
    • 84876921975 scopus 로고    scopus 로고
    • 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)
    • 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).
  • 36
    • 84876900883 scopus 로고    scopus 로고
    • 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
    • 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).
  • 37
    • 84876936682 scopus 로고    scopus 로고
    • 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
    • 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).


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.