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Single Crystals of a 2-Dimensional Metal Coordination Polymer Containing Pendant Carbazole Groups
Single Crystals of a 2-Dimensional Metal Coordination Polymer Containing Pendant Carbazole Groups
Bulletin of the Korean Chemical Society. 2013. Dec, 34(12): 3903-3905
Copyright © 2013, Korea Chemical Society
  • Received : August 20, 2013
  • Accepted : September 25, 2013
  • Published : December 20, 2013
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About the Authors
Eun-Young Choi
Korea Science Academy of KAIST, Busan 614-822, Korea
Sang-Beom Lee
Department of Molecular Science and Technology, Ajou University, Suwon 443-749, Korea.
Hoseop Yun
Department of Chemistry & Division of Energy Systems Research, Ajou University, Suwon 443-749, Korea
Suck-Hyun Lee
Department of Molecular Science and Technology, Ajou University, Suwon 443-749, Korea.
Chunji Gao
Department of Molecular Science and Technology, Ajou University, Suwon 443-749, Korea.
Youngmu Shin
Korea Science Academy of KAIST, Busan 614-822, Korea
O-Pil Kwon
Department of Molecular Science and Technology, Ajou University, Suwon 443-749, Korea.

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Experimental Section
Synthesis of Monomer. The organic linker CZ3-acid was synthesized by a method that was similar to that described in Ref. [28]. 1 H-NMR (400 MHz, DMSO- d 6 , δ relative to (CH 3 ) 4 Si): 1 H-NMR (400 MHz, DMSO- d 6 ) δ 8.11 (d, 4H, J = 7.6 Hz, C 6 H 4 ), 7.61 (d, 4H, J = 8.0 Hz, C 6 H 4 ), 7.36 (t, 4H, J = 15.2 Hz, C 6 H 4 ), 7.29 (s, 2H, C 6 H 2 ), 7.15 (t, 4H, J = 14.8 Hz, C 6 H 4 ), 4.58 (t, 4H, J = 14.0 Hz, CH 2 ), 3.99 (t, 4H, J = 10.8 Hz, CH 2 ), 2.16 (t, 4H, J = 11.2 Hz, CH 2 ).
Synthesis of Polymer. The metal coordination polymer was synthesized by a solvothermal reaction; 15 the organic linker CZ3-acid (0.125 mmol, 0.0766 g) and Zn(NO 3 ) 2 ·6H 2 O (0.25 mmol, 0.0744 g) were added to a solvent mixture containing 2 mL of dimethylformamide (DMF) and 2 mL of ethanol, and heated to 100 °C for 1 day. Needle-like crystals were obtained. There were filtered and washed with DMF and acetone. The synthesis of metal coordination polymer was very sensitive to the ratio of solvent mixture and other experimental conditions and then easily formed another crystalline powders. The yield of [Zn(CZ3)(DMF)] phase is obtained up to 65%.
Crystal Structure Analysis : C 41 H 37 N 3 O 7 Zn, M r =749.1, triclinic, space group P-1 , a = 10.0375 (5) Å, b = 10.3460 (4) Å, c = 18.1680 (8) Å, α= 87.3327 (11)°, β = 83.8644 (12)°, γ = 77.4709 (13)°, V = 1830.70 (14) Å 3 , Z = 2, T = 290 (1) K, μ (Mo Ka) = 0.73 mm −1 . Of 14369 reflections collected in the θ range 3.0 o -25.0 o using w scans on a Rigaku R-axis Rapid S diffractometer, 6423 were unique reflections ( R int = 0.028). The structure was solved and refined against F 2 using SHELX-97, 29 469 variables, R 1 = 0.035 (F o 2 > 2σ(F o 2 )), wR 2 = 0.108, GOF = 1.19, and max/min residual electron density 0.76/−0.96 eÅ −3 . CCDC-950341.
Acknowledgements
This work has been supported by Midcareer Researcher Program (NRF-2013R1A2A2A01007232) and Basic Science Research Program (2009-0093826) through the National Research Foundation of Korea (NRF) funded by the Korea government.
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