Controlled synthesis of large single crystals of metal‐organic framework CPO‐27‐Ni prepared by a modulation approach: in situ single crystal X‐ray diffraction studies

DOI: 10.1002/chem.202100528
Data DOI: 10.17630/91fe66c8-7754-4a92-9af1-ab0f5dab8e22

Authors: Simon Maximilian Vornholt (University of St Andrews) , Caroline Elliott (University of St Andrews) , Cameron Rice (University of St Andrews) , Samantha Russell (University of St Andrews) , Peter J. Kerr (University of St Andrews) , Daniel N. Rainer (University of St Andrews) , Michal Mazur (Charles University) , Mark R. Warren (Diamond Light Source) , Paul S. Wheatley (University of St Andrews) , Russell E. Morris (University of St Andrews)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Chemistry – A European Journal

State: Published (Approved)
Published: March 2021
Diamond Proposal Number(s): 24028

Abstract: The size of single crystals of the metal-organic framework CPO-27-Ni was incrementally increased through a series of modulated syntheses. A novel linker modulated synthesis using 2,5-dihydroxyterephthalic acid and the isomeric ligand 4,6-dihydroxyisophthalic acid yielded large single crystals of CPO-27-Ni (~70 µm). All materials proved high crystallinity and phase pure through powder X-ray diffraction, electron microscopy methods, thermogravimetric, and compositional analysis. For the first time single crystal structure analyses were carried out on CPO-27-Ni. High BET surface areas and nitric oxide (NO) release efficiencies were recorded for all materials. Large single crystals of CPO-27-Ni showed a prolonged NO release and proved suitable for in situ single crystal diffraction experiments to follow the NO adsorption. An efficient activation protocol was developed, leading to a dehydrated structure after just 4 h, which subsequently was NO-loaded, giving a first NO loaded single crystal structural model of CPO-27-Ni.

Journal Keywords: CPO-27-M; gas adsorption; metal-organic frameworks; modulation synthesis; MOF-74; single crystals

Subject Areas: Materials, Chemistry


Instruments: I19-Small Molecule Single Crystal Diffraction

Added On: 30/03/2021 22:20

Discipline Tags:

Chemistry Materials Science Metal-Organic Frameworks Life Sciences & Biotech Metallurgy Organometallic Chemistry

Technical Tags:

Diffraction Single Crystal X-ray Diffraction (SXRD)