Synthesis and crystallographic characterisation of Mg(H 2 dhtp)(H 2 O) 5 ·H 2 O

Henkelis, Susan E.; McCormick, Laura J.; Cordes, David B.; Slawin, Alexandra M. Z.; Morris, Russell E.

doi:10.1016/j.inoche.2016.01.007

Cited by 15 publications

(11 citation statements)

References 27 publications

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“…Other studies on the synthesis of CPO‐27‐M have identified monomeric species as competing phases in the synthesis, proving that this framework is sensitive towards slight changes in the reaction conditions [49,57,58] . As we only observe the formation of a single phase, we propose that CPO‐27‐Ni is the thermodynamic product under these synthesis conditions and the presence of a competing linker promotes crystal growth through nucleation.…”

Section: Resultssupporting

confidence: 60%

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

Vornholt

Elliott

Rice

et al. 2021

Chemistry A European J

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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.

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Section: Resultssupporting

confidence: 60%

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

Vornholt

Elliott

Rice

et al. 2021

Chemistry A European J

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“…Compound 2 was readily obtained by LAG (10 minutes) using equimolar amounts of MgO with H4dhta in presence of water (η= 0.95 μL/mg and 0.85 μL/mg for MgZn-and MgCo-MOF-74, respectively). Complete conversion to 2 was evidenced by PXRD patterns measured for the milled reaction mixture exhibiting Bragg reflections consistent with the known crystal structure of 2 (CSD code XAJGEX), 58 and lack reflections for any of the reactants (Fig. 4).…”

Section: Introductionsupporting

confidence: 60%

“…Importantly, using oxides and acetates as a metal source is an environmentally-friendly alternative to conventional synthesis of MOFs that often requires toxic and corrosive metal precursors such as chloride and nitrates. were previously reported, 58,59 while the structures of 3 and 4 are determined here using single crystal and powder X-ray diffraction (PXRD) data, respectively (see SI). We first explored our strategy by using 1 as a precursor in a set of LAG mechanochemical reactions involving an equimolar amount of either MgO, CoCO3 or Cu(OH)2.…”

Section: Introductionmentioning

confidence: 93%

Rational Synthesis of Mixed-Metal Microporous Metal–Organic Frameworks with Controlled Composition Using Mechanochemistry

et al. 2019

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Metal-Organic Frameworks Using Pre-Assembled Precursors. ChemRxiv. Preprint. Ball milling mechanochemistry enables enables targeted, rapid synthesis of mixed-metal metal-organic frameworks (MOFs) with controllable stoichiometric composition. Specifically, the use of ball milling enabled the use of pre-assembled coordination polymers of zinc, magnesium, nickel(II) and cobalt(II) as precursors in an innovative mechanochemical strategy for the deliberate assembly of mixed-metal MOF-74 materials comprised of pairs of transition of main group metals in a pre-determinmed 1:1 stoichiometric ratio, including ZnMg-, ZnCo, ZnCu, MgZn-, MgCo-, MgCa-, NiZn-,NiMg-, NiCo-, CoZn-, CoMg-and CoCu-MOF-74. While this is the first example of target-oriented MOF synthesis using mechanochemistry, it also provides an entry to controlling the stoichiometric composition of mixed-metal frameworks. File list (2) download file view on ChemRxiv manuscript_ChemRxiv.pdf (1.09 MiB) download file view on ChemRxiv SI_ChemRxiv.pdf (2.25 MiB) Mechanochemistry enables targeted synthesis of mixed-metal microporous metal-organic frameworks using pre-assembled precursors

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“…43−45 RE elements such as europium and terbium are known to preferentially bind to acid gases such as NO x . 46 A well-known family of MOFs, M-MOF-74 (CPO-27, M 2 DOBDC), consists of a DOBDC linker connected by transition metal ions (Co, 47 Cu, 48 Mg, 29,47,49,50 Mn, 51 Ni, 29,47,52,53 and Zn) 54,55 to form a three-dimensional porous structure with hexagonal 14 Å pores and an internal pore surface area of between 1039 and 1052 m 2 g −1 . 47 Upon activation to remove bound solvent molecules, these MOFs are able to form one coordinatively unsaturated site (CUS) per metal center.…”

Section: ■ Introductionmentioning

confidence: 99%

Preferential SO_x Adsorption in Mg-MOF-74 from a Humid Acid Gas Stream

Henkelis

Judge

Hayes

et al. 2021

ACS Appl. Mater. Interfaces

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The preferential adsorption of SO x versus water in Mg-MOF-74 from a humid SO x gas stream has been investigated via materials studies and nuclear magnetic resonance (NMR). Mg-MOF-74 has been synthesized and subsequently loaded simultaneously with water vapor and SO x (62–96 ppm) in an adsorption chamber at room temperature over a time period of 4 days with a sample taken every 24 h. Each sample was analyzed by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA)–mass spectrometry, and scanning electron microscopy–energy-dispersive spectroscopy. The metal–organic framework (MOF) showed retained crystallinity and peak intensity in PXRD, and after 2 days, it showed no obvious degradation to the structure. Use of multiple techniques, including TGA, identified 10% by weight of SO x species, specifically H2S and SO2, within the MOF. 1H solid-state NMR shows a substantial reduction of H2O when SO x is present, which is consistent with SO x preferentially binding to the oxophilic metal site of the framework. After 14 weeks aging, the sulfur remains present in the three-dimensional MOF, with only half being desorbed after 23 weeks in air.

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Synthesis and crystallographic characterisation of Mg(H 2 dhtp)(H 2 O) 5 ·H 2 O

Cited by 15 publications

References 27 publications

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

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

Rational Synthesis of Mixed-Metal Microporous Metal–Organic Frameworks with Controlled Composition Using Mechanochemistry

Preferential SO_x Adsorption in Mg-MOF-74 from a Humid Acid Gas Stream

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Synthesis and crystallographic characterisation of Mg(H 2 dhtp)(H 2 O) 5 ·H 2 O

Cited by 15 publications

References 27 publications

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

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

Rational Synthesis of Mixed-Metal Microporous Metal–Organic Frameworks with Controlled Composition Using Mechanochemistry

Preferential SOx Adsorption in Mg-MOF-74 from a Humid Acid Gas Stream

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Preferential SO_x Adsorption in Mg-MOF-74 from a Humid Acid Gas Stream