Cost-effective 17O enrichment of metal–organic frameworks enables the composition and disorder in mixed-metal materials to be determined using NMR spectroscopy.

ABSTRACT:The hydrothermal synthesis of a zeolite, with properties suitable for use in the ADOR (AssemblyDisassembly-Organisation-Reassembly) process, has been designed and a zeolite, called SAZ-1, successfully prepared. This zeolite has then been used as a parent in the ADOR process and two new daughter zeolites, IPC-15 and IPC-16, have been prepared. The X-ray powder diffraction patterns of the new zeolites match well those predicted using computational methods. The three materials, form an isoreticular series with decreasing pores size from 14-ring to 12-ring to 10-ring.

The assembly–disassembly–organization–reassembly (ADOR) process has been used to disassemble a parent zeolite with the UOV structure type and then reassemble the resulting layers into a novel structure, IPC‐12. The structure of the material has previously been predicted computationally and confirmed in our experiments using X‐ray diffraction and atomic resolution STEM‐HAADF electron microscopy. This is the first successful application of the ADOR process to a material with porous layers.

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 were shown to have high crystallinity and phase purity through powder X‐ray diffraction, electron microscopy methods, thermogravimetry, 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, leading to a first NO loaded single‐crystal structural model of CPO‐27‐Ni.