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Crystal structure of 1-propanethiol–Co2(dobdc) from laboratory X-ray powder diffraction data

Published online by Cambridge University Press:  10 February 2020

Jonathan B. Lefton ,
Kyle B. Pekar ,
Daniel Sethio ,
Elfi Kraka  and
Tomče Runčevski Open the ORCID record for Tomče Runčevski [Opens in a new window]
Jonathan B. Lefton
Affiliation:
Department of Chemistry, Southern Methodist University, Dallas, TX75275, USA
Kyle B. Pekar
Affiliation:
Department of Chemistry, Southern Methodist University, Dallas, TX75275, USA
Daniel Sethio
Affiliation:
Department of Chemistry, Southern Methodist University, Dallas, TX75275, USA
Elfi Kraka
Affiliation:
Department of Chemistry, Southern Methodist University, Dallas, TX75275, USA
Tomče Runčevski*
Affiliation:
Department of Chemistry, Southern Methodist University, Dallas, TX75275, USA
*
a)Author to whom correspondence should be addressed. Electronic mail: truncevski@smu.edu
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Abstract

Laboratory X-ray powder diffraction was used to solve and refine the crystal structures of appended guest molecules within the pores of metal–organic frameworks (MOFs). Herein, we report the crystal structure of 1-propanethiol adsorbed in the pores of Co2(dobdc) (dobdc4– = 2,5-dioxido-1,4-benzenedicarboxylate, MOF-74). Soaking the activated MOF in neat 1-propanethiol resulted in the formation of 1-propanethiol–Co2(dobdc). The thiol appendant MOF maintained the crystal symmetry, with a rhombohedral space group R-3 and unit-cell parameters a = 25.9597(9) Å, c = 6.8623(5) Å, and V = 4005.0(4) Å3. As expected, the thiol sulfur formed a bond with the open cobalt metal site. The alkane chain was directed toward the center of the pore, participating in numerous van der Waals weak interactions with neighboring molecules. For the final Rietveld refinement, soft restrains were applied using bond distances obtained by periodic density functional theory (DFT) geometry optimization.

Keywords

MOFX-ray powder diffractioncrystal structureRietveld refinementgeometry optimization
Type
Invited Paper
Information
Powder Diffraction , Volume 35 , Issue 1 , March 2020 , pp. 3 - 6
Copyright
Copyright © International Centre for Diffraction Data 2020

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