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Near-critical water, a cleaner solvent for the synthesis of a metal-organic framework

DOI: 10.1039/c1gc15726d DOI Help

Authors: Ilich A. Ibarra (University of Nottingham) , Peter Bayliss (University of Nottingham) , Eduardo Perez (University of Nottingham) , Sihai Yang (University of Nottingham) , Alexander J. Blake (University of Nottingham) , Harriott Nowell (Diamond Light Source) , Martyn Poliakoff (University of Nottingham) , Martin Schroeder (University of Nottingham) , David R. Allan (Diamond Light Source)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Green Chemistry

State: Published (Approved)
Published: November 2011
Diamond Proposal Number(s): 6410

Abstract: The microporous metal–organic framework {[Zn2(L)]·(H2O)3}? (H4L = 1,2,4,5-tetrakis(4-carboxyphenyl)benzene) has been synthesised using near-critical water (300 °C) as a cleaner alternative to toxic organic solvents. A single crystal X-ray structure determination confirms that the complex incorporates tetrahedral Zn(II) centres bridged through the carboxylate anions to form a binuclear building block, which extends into a one dimensional chain along the c axis. Four L4? ligands bind to each Zn(II) centre and cross-link the one dimensional chains along both a and b axes to afford a three dimensional network structure incorporating pores of ca. 4.3 Å in diameter. The complex shows high thermal stability up to 425 °C by gravimetric thermal analysis, and on desolvation, displays a high adsorption enthalpy of 11.0 kJ mol?1 for H2 uptake at zero coverage, consistent with the narrow pore diameter for the framework.

Journal Keywords: Mof; Clean Solvent; Synthesis; Environment

Diamond Keywords: Hydrogen Storage

Subject Areas: Chemistry, Materials, Energy

Instruments: I19-Small Molecule Single Crystal Diffraction

Added On: 30/09/2011 20:00

Discipline Tags:

Energy Storage Energy Chemistry Materials Science Metal-Organic Frameworks Metallurgy Organometallic Chemistry

Technical Tags:

Diffraction Single Crystal X-ray Diffraction (SXRD)