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

Simon Maximilian Vornholt; Caroline Elliott; Cameron M. Rice; Samantha E. Russell; Peter J. Kerr; Daniel N. Rainer; Michal Mazur; Mark R. Warren; Paul S. Wheatley; Russell E. Morris

doi:10.1002/chem.202100528

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

Simon Maximilian Vornholt^*, Caroline Elliott, Cameron M. Rice, Samantha E. Russell, Peter J. Kerr, Daniel N. Rainer, Michal Mazur, Mark R. Warren, Paul S. Wheatley, Russell E. Morris

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

8 Citations (Scopus)

19 Downloads (Pure)

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 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.

Original language	English
Pages (from-to)	8537-8546
Number of pages	11
Journal	Chemistry - A European Journal
Volume	27
Issue number	33
Early online date	7 May 2021
DOIs	https://doi.org/10.1002/chem.202100528
Publication status	Published - 10 Jun 2021

Keywords

CPO-27
Gas adsorption
Metal-organic frameworks (MOFs)
Modulation synthesis
MOF-74
Single crystals

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10.1002/chem.202100528Licence: CC BY

Vornholt_2021_CEJ_Controlled_CC
Copyright © 2021 The Authors. Chemistry - A European Journal published by Wiley-VCH GmbH. This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited.
Final published version, 1.44 MBLicence: CC BY

H2020 ERC Advanced Grant 2017 ADOR: H2020 ERC Advanced Grant 2017 ADOR
Morris, R. E. (PI)
European Research Council
1/10/18 → 30/09/23
Project: Fellowship
CRITICAT Equipment Account: CRITICAT Equipment Fund
Smith, A. D. (PI)
EPSRC
21/07/14 → 30/06/15
Project: Standard
CRITICAT CDT: Critical Resource Catalysis - CRITICAT
Smith, A. D. (PI), Nolan, S. P. (CoI) & Westwood, N. J. (CoI)
EPSRC
1/05/14 → 31/10/22
Project: Standard

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 (dataset)
Vornholt, S. M. (Creator), Elliott, C. (Creator), Rice, C. M. (Creator), Russell, S. E. (Creator), Kerr, P. J. (Creator), Rainer, D. N. (Creator), Mazur, M. (Creator), Warren, M. R. (Creator), Wheatley, P. S. (Creator) & Morris, R. E. (Creator), University of St Andrews, 10 May 2021
DOI: 10.17630/91fe66c8-7754-4a92-9af1-ab0f5dab8e22
Dataset

File
CCDC 2060146 & 2060150 - 2060152: Experimental Crystal Structure Determination
Vornholt, S. M. (Creator), Elliott, C. G. (Creator), Rice, C. M. (Creator), Russell, S. E. (Creator), Kerr, P. J. (Creator), Rainer, D. N. (Creator), Mazur, M. (Creator), Warren, M. R. (Creator), Wheatley, P. S. (Creator) & Morris, R. E. (Creator), Cambridge Crystallographic Data Centre, 2021
DOI: 10.5517/ccdc.csd.cc274rbh, https://dx.doi.org/10.5517/ccdc.csd.cc274rgm and 2 more links, https://dx.doi.org/10.5517/ccdc.csd.cc274rhn, https://dx.doi.org/10.5517/ccdc.csd.cc274rjp (show fewer)
Dataset

Cite this

Vornholt, S. M., Elliott, C., Rice, C. M., Russell, S. E., Kerr, P. J., Rainer, D. N., Mazur, M., Warren, M. R., Wheatley, P. S., & Morris, R. E. (2021). 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. Chemistry - A European Journal, 27(33), 8537-8546. https://doi.org/10.1002/chem.202100528

@article{df7f0fa222644ebeabf85a4590b5951e,

title = "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",

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 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.",

keywords = "CPO-27, Gas adsorption, Metal-organic frameworks (MOFs), Modulation synthesis, MOF-74, Single crystals",

author = "Vornholt, {Simon Maximilian} and Caroline Elliott and Rice, {Cameron M.} and Russell, {Samantha E.} and Kerr, {Peter J.} and Rainer, {Daniel N.} and Michal Mazur and Warren, {Mark R.} and Wheatley, {Paul S.} and Morris, {Russell E.}",

note = "The authors would like to thank EPSRC Capital for Great Technologies grant (EP/L017008/1) for supporting electron microscopy facilities at the University of St Andrews. S.M.V. and S.E.R. acknowledge the European Research Council for funding opportunities under grant agreement no. 787073. The authors C.M.R., D.N.R., C.G.E., and S.M.V. would like to thank the EPSRC for funding opportunities (C.M.R. & D.N.R. - EP/N509759/1; C.G.E. - EP/L016419, S.M.V. - EP/K005499/1). M.M. and R.E.M. would like to thank the OP VVV {"}Excellent Research Teams{"}, project no. CZ.02.1.01/0.0/0.0/15_003/0000417-CUCAM. ",

year = "2021",

month = jun,

day = "10",

doi = "10.1002/chem.202100528",

language = "English",

volume = "27",

pages = "8537--8546",

journal = "Chemistry - A European Journal",

issn = "0947-6539",

publisher = "John Wiley & Sons, Ltd",

number = "33",

}

Vornholt, SM, Elliott, C, Rice, CM, Russell, SE, Kerr, PJ, Rainer, DN, Mazur, M, Warren, MR, Wheatley, PS & Morris, RE 2021, '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', Chemistry - A European Journal, vol. 27, no. 33, pp. 8537-8546. https://doi.org/10.1002/chem.202100528

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, Simon Maximilian; Elliott, Caroline; Rice, Cameron M. et al.
In: Chemistry - A European Journal, Vol. 27, No. 33, 10.06.2021, p. 8537-8546.

Research output: Contribution to journal › Article › peer-review

TY - JOUR

T1 - Controlled synthesis of large single crystals of metal-organic framework CPO-27-Ni prepared by a modulation approach

T2 - in situ single crystal X-ray diffraction studies

AU - Vornholt, Simon Maximilian

AU - Elliott, Caroline

AU - Rice, Cameron M.

AU - Russell, Samantha E.

AU - Kerr, Peter J.

AU - Rainer, Daniel N.

AU - Mazur, Michal

AU - Warren, Mark R.

AU - Wheatley, Paul S.

AU - Morris, Russell E.

N1 - The authors would like to thank EPSRC Capital for Great Technologies grant (EP/L017008/1) for supporting electron microscopy facilities at the University of St Andrews. S.M.V. and S.E.R. acknowledge the European Research Council for funding opportunities under grant agreement no. 787073. The authors C.M.R., D.N.R., C.G.E., and S.M.V. would like to thank the EPSRC for funding opportunities (C.M.R. & D.N.R. - EP/N509759/1; C.G.E. - EP/L016419, S.M.V. - EP/K005499/1). M.M. and R.E.M. would like to thank the OP VVV "Excellent Research Teams", project no. CZ.02.1.01/0.0/0.0/15_003/0000417-CUCAM.

PY - 2021/6/10

Y1 - 2021/6/10

N2 - 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.

AB - 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.

KW - CPO-27

KW - Gas adsorption

KW - Metal-organic frameworks (MOFs)

KW - Modulation synthesis

KW - MOF-74

KW - Single crystals

U2 - 10.1002/chem.202100528

DO - 10.1002/chem.202100528

M3 - Article

SN - 0947-6539

VL - 27

SP - 8537

EP - 8546

JO - Chemistry - A European Journal

JF - Chemistry - A European Journal

IS - 33

ER -

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

Abstract

Keywords

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Projects

H2020 ERC Advanced Grant 2017 ADOR: H2020 ERC Advanced Grant 2017 ADOR

CRITICAT Equipment Account: CRITICAT Equipment Fund

CRITICAT CDT: Critical Resource Catalysis - CRITICAT

Datasets

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 (dataset)

CCDC 2060146 & 2060150 - 2060152: Experimental Crystal Structure Determination

Cite this