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Macrocyclic Zinc(II) Coordination Polymers Constructed from Aromatic and Cyclohexane Dicarboxylate Ligands
Macrocyclic Zinc(II) Coordination Polymers Constructed from Aromatic and Cyclohexane Dicarboxylate Ligands
Journal of the Korean Chemical Society. 2015. Aug, 59(4): 336-340
Copyright © 2015, Korean Chemical Society
  • Received : April 14, 2015
  • Accepted : May 08, 2015
  • Published : August 31, 2015
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About the Authors
Taeyeong Kim
Jin Suk Kwag
Ju Chang Kim
E-mail:kimjc@pknu.ac.kr

Abstract
Keywords
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EXPERIMENTAL
- Materials, Methods and Apparatus
All commercially available chemicals were used as received. Water was distilled before use. IR spectra of solid samples (KBr pellets) were recorded on a Perkin-Elmer Spectrum X spectrophotometer between 4000 cm −1 and 400 cm −1 . The elemental analyses (C, H, N) were performed on samples using a CE Instruments EA-1110 Elemental Analyzer at KRICT, Korea. The free ligand L1 , Zn( L1 )(NO 3 ) 2 and Na 2 bpdc were synthesized by literature procedures. 24,26,27
- Synthesis of 1
To a DMF (10 mL) solution of Zn( L1 )(NO 3 ) 2 (53 mg, 0.1 mmol) was added a stoichiometric amount of Na 2 bpdc (29 mg, 0.1 mmol) in water (10 mL), which was allowed to stand in an open beaker at ambient temperature. After a week, colorless crystals of 1 were obtained. Yield: >90% based on Zn( L1 )(NO 3 ) 2 . Anal. Calcd. for C 34 H 49.50 ZnN 4 O 4.75 (2): C, 62.29%; H, 7.61%; N, 8.55%. Found C, 62.69%; H, 7.57%; N, 8.66%. IR (KBr, cm −1 ): 3491, 3345 (νOH), 3220, 3125 (νNH), 1592, 1540 (ν as COO), 1380 (ν s COO).
- Synthesis of 2
To a DMF (10 mL) solution of Zn( L1 )(NO 3 ) 2 (263 mg, 0.5 mmol) was added an aqueous solution of e,e-trans -1,4-chdcH 2 (86 mg, 0.5 mmole) and five pipette drops of triethylamine. The mixture was left until colorless blocks of 2 formed. The crystals were filtered and dried in air. Yield: 67% based on Zn( L1 )(NO 3 ) 2 . Anal. Calc. for C 28 H 54 N 4 O 6 Zn-2H 2 O: C, 58.72%; H, 8.74%; N, 9.79%. Found C, 58.75%; H, 8.91%; N, 9.88%. IR (KBr, cm −1 ): 3413 (νOH), 3160 (νNH), 1649 (δH 2 O), 1572 (ν as COO), 1384 (ν s COO).
- X-ray Crystallography
5 contains a summary of selected crystallographic data and structure refinement details for 1 and 2 . Data were collected on a Nonius Kappa CCD (for 1 ) or a Bruker Kappa APEX-DUO CCD (for 2 ) diffractometer, using graphite monochromated Mo K α radiation. A combination of ϕ and ω (with κ offsets) scans were used to collect sufficient data. The Denzo-SMN package was used to process the data frames. 28 The structures were solved and refined using the SHELXTL∖PC V6.1 package. 29 Refinement was performed by full-matrix least squares on F 2 using all data (negative intensities included). Crystallographic data for the structures reported here have been deposited with CCDC (Deposition Nos. CCDC-743544 ( 1 ) and CCDC-1059162 ( 2 )). These data can be obtained free of charge via http://www.ccdc.cam.ac.uk/conts/retrieving.html or from CCDC, 12 Union Road, Cambridge CB2 1EZ, UK, E-mail: deposit@ccdc.cam.ac.uk
Crystal data and structure refinement for1and2
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Crystal data and structure refinement for 1 and 2
Supporting Information. IR spectra and TGA curves for the complexes 1 and 2 are available ( Figures S1–S4).
Acknowledgements
This work was supported by the Pukyong National University Research Fund (2014). Authors are grateful to Dr. Alan J. Lough at University of Toronto for assistance with X-ray crystallography.
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