Advanced
Structural Transformation and Gas Adsorption Properties of Interpenetrated IRMOF-8
Structural Transformation and Gas Adsorption Properties of Interpenetrated IRMOF-8
Bulletin of the Korean Chemical Society. 2014. Mar, 35(3): 949-952
Copyright © 2014, Korea Chemical Society
  • Received : September 23, 2013
  • Accepted : September 30, 2013
  • Published : March 20, 2014
Download
PDF
e-PUB
PubReader
PPT
Export by style
Article
Author
Metrics
Cited by
TagCloud
About the Authors
Jang-Hoon Cho
Sang Moon Lee
Division of Materials Science, Korea Basic Science Institute, Daejeon 305-333, Korea
Jong Won Shin
Dohyun Moon
Pohang Accelerator Laboratory, Pohang, Kyungbook 790-784, Korea
Kil Sik Min
Myoung Soo Lah
Interdisciplinary School of Green Energy, Ulsan National Institute of Science and Technology, Ulsan 689-798, Korea
Hong-In Lee

Abstract
Keywords
PPT Slide
Lager Image
PPT Slide
Lager Image
PPT Slide
Lager Image
PPT Slide
Lager Image
PPT Slide
Lager Image
Experimental
Synthesis. INT-IRMOF-8-A was synthesized solvothermally. Zn(NO 3 ) 2 ·6H 2 O (0.17 g, 0.57 mmol) and 2,6-naphthalenedicarboxylic acid (H 2 NDC, 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 Zn 4 O(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 N 2 flow. Powder X-ray diffraction (PXRD) data were measured on a Shimadzu XRD 600 using Cu K α1 radiation (λ = 1.5418 Å). The numerical PXRD simulations were performed using Mercury 3.1 software. N 2 and H 2 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 MoK α 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
Acknowledgements
This research was supported by Basic Science Research Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education, Science and Technology (2013-053145).Supporting Information.Thermogravimetric analysis data, crystal data and structure refinements are included in supporting information.
References
Stock N. , Biswas N. 2012 Chem. Rev. 112 933 - 969
Wang C. , Zhang T. , Lin W. 2012 Chem. Rev. 112 1084 - 1104
Li J.-R. , Sculley J. , Zhou H.-C. 2012 Chem. Rev. 112 869 - 932
Kreno J. E. , Leong K. , Farha O. K. , Allendorf M. , Van Duyne R. P. , Hupp J. T. 2012 Chem. Rev. 112 1105 - 1125
Suh M. P. , Park H. J. , Prasad T. K. , Lim D.-W. 2012 Chem. Rev. 112 782 - 835
Yaghi O. M. , O'Keeffe M. 2012 Chem. Rev. 112 675 - 702
Gu Z.-Y. , Yang C.-X. , Chang N. , Yan X.-P. 2012 Acc. Chem. Res. 45 734 - 735
Eddaoudi M. , Kim J. , Rosi N. , Vodak D. , Wachter J. , O'Keeffe M. , Yaghi O. M. 2002 Sicence 295 469 - 472
Rosi N. L. , Eckert J. , Eddaoudi M. , Vodak D. T. , Kim J. , O'Keeffe M. , Yaghi O. M. 2003 Sicence 300 1127 - 1129
Yaghi O. M. , Eddaoudi M. , Li H. , Kim J. , Rosi N. 2005 6930193 B2 US Pat.
Siberio-Perez D. Y. , Wong-Foy A. G. , Yaghi O. M. , Matzger A. J. 2007 Chem. Mater. 19 3681 - 3685
Yao Q. , Su J. , Cheung O. , Liu Q. , Hedin N. , Zou X. 2012 J. Mater. Chem. 22 10345 - 10351
Perry IV J. J. , Feng P. L. , Meek S. T. , Leong K. , Doty F. P. , Allendorf M. P. 2012 J. Mater. Chem. 22 10235 - 10248
Nguyen L. T. L. , Nguyen C. V. , Dang G. H. , Le K. K. A. , Phan N. T. S. 2011 J. Mol. Cat. A: Chem. 349 28 - 35
Orefuwa S. A. , Yang H. , Goudy A. J. 2012 Micropor. Mesopor. Mater. 153 88 - 93
Rowsell J. L. C. , Millward A. R. , Park K. S. , Yaghi O. M. 2004 J. Am. Chem. Soc. 126 5666 - 5667
Li Y. , Yang R. T. 2006 J. Am. Chem. Soc. 128 726 - 727
Sheldrick G. M. 1997 SHELXTL-PLUS, Crystal Structure Analysis Package, Bruker Analytical X-Ray Madison, WI, USA
Spek A. L. 2003 J. Appl. Crystallogr. 36 7 - 13