Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
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Structural Transformation and Gas Adsorption Properties of Interpenetrated IRMOF-8

  • Cho, Jang-Hoon (Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University) ;
  • Lee, Sang Moon (Division of Materials Science, Korea Basic Science Institute) ;
  • Shin, Jong Won (Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University) ;
  • Moon, Dohyun (Pohang Accelerator Laboratory) ;
  • Min, Kil Sik (Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University) ;
  • Lah, Myoung Soo (Interdisciplinary School of Green Energy, Ulsan National Institute of Science and Technology) ;
  • Lee, Hong-In (Department of Chemistry and Green-Nano Materials Research Center, Kyungpook National University)
  • Received : 2013.09.23
  • Accepted : 2013.09.30
  • Published : 2014.03.20
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Abstract

Keywords

Experimental

Synthesis. INT-IRMOF-8-A was synthesized solvothermally. Zn(NO3)2·6H2O (0.17 g, 0.57 mmol) and 2,6-naphthalenedicarboxylic acid (H2NDC, 0.06 g, 0.28 mmol) were dissolved in a mixed solvent of DMF (10 mL) and 1,4- dioxane (2 mL) and stirred for 2 h at room temperature. The resulting solution was sealed in a teflon-capped scintillation vial for 24 h at 110 ℃. Colorless crystals were filtered to be collected and washed three times with a mixed solvent of DMF and 1,4-dioxane. The crystals were dried in vacuum evaporator for 2 h. Yield: 95%. The chemical formula for the activated INT-IRMOF-8-A is Zn4O(NDC)3, as derived from the structural refinement and elemental analysis. Calculated (%): C 47.00, H 1.97, N 0.0. Found (%): C 46.45, H 1.84, N 0.0. INT-IRMOF-8-B was synthesized similarly in a mixed solvent of DMF (12 mL) and formic acid (100 mL).

INT-IRMOF-8-C was obtained from INT-IRMOF-8-A. INT-IRMOF-8-A was placed in ethanol solvent at room temperature for 3 days and dried in vacuum for 2 h. Colorless crystals were collected for single crystal analysis.

Physical Measurements. Elemental analysis (EA) was performed using a Perkin-Elmer 2400 CHN analyzer. Thermogravimetric analysis (TGA) was performed on a Seiko TG/ DTA 320. The samples were heated from 30 to 800 ℃ with 10 ℃/min scan speed under N2 flow. Powder X-ray diffraction (PXRD) data were measured on a Shimadzu XRD 600 using Cu Kα1 radiation (λ = 1.5418 Å). The numerical PXRD simulations were performed using Mercury 3.1 software. N2 and H2 adsorption–desorption isotherms were collected at 77 K and/or 88 K with a standard static volumetric technique on a Micromeritics ASAP2010 analyzer. The isotherms of the MOFs were recorded after chloroform exchange and degassing under vacuum for 6 h at 100 ℃.

X-ray Crystallography. X-ray diffraction data for INTIRMOF- 8-A and INT-IRMOF-8-C were collected on a 4AMXW ADSC Quantum-210 detector with a Pt-coated Si double crystal monochromator (λ = 0.77000 Å for INTIRMOF- 8-A and λ = 0.90000 Å for INT-IRMOF-8-C) at 100(2) K in Pohang Accelerator Laboratory (PAL), Korea. X-ray diffraction data for INT-IRMOF-8-B were collected on a Bruker SMART APEXII diffractometer equipped with graphite monochromated MoKα radiation (λ = 0.71073 Å) at 200(2) K in Korea Basic Science Institute. The crystal structures were solved by the direct method and refined by fullmatrix least-squares calculation with the SHELXTL software package.19 The positions of all non-hydrogen atoms were refined with anisotropic displacement factors. However, due to the disorder, carbon atom (C24) of the 2,6-naphthalenedicarboxylate (NDC) anion was refined isotropically in INTIRMOF- 8-B. All hydrogen atoms were theoretically added and included in the final refinement. The final refinement was performed with modification of the structure factors for contribution of the disordered solvent electron densities using the PLATON/SQUEEZE program.20 Crystal data and structure refinements are listed in table S1. Crystallographic data for the structures reported in this paper have been deposited with Cambridge Crystallographic Data Centre (Deposition No. CCDC-957268 for INT-IRMOF-8-A, CCDC- 957270 for INT-IRMOF-8-B, and CCDC-957269 for INTIRMOF- 8-C). These data can be obtained free of charge from the Cambridge Crystallographic Data Centre via http:// www.ccdc.cam.ac.uk/conts/retrieving.html

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