Journal
CRYSTAL GROWTH & DESIGN
Volume 19, Issue 4, Pages 2089-2096Publisher
AMER CHEMICAL SOC
DOI: 10.1021/acs.cgd.8b01657
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Funding
- Research Council of Norway through the FRINATEK program [221596]
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Electrospray ionization mass spectrometry (ESI-MS) has been utilized to investigate the self-assembly processes occurring during the formation of the microporous metal-organic framework CPO-27-M (M = Co, Ni). The mono- and dinuclear building units {M(H(x)dhtp)} and {M-2(H(x)dhtp)}, where Hxdhtp is the organic linker HxC8O6 and fragments thereof, were identified as key species present in the reaction mixture during the product formation. Time-resolved powder X-ray diffraction analysis was used to follow the synthesis and confirmed that no other crystalline products occur in the reaction mixture prior to the crystallization of CPO-27-Ni. When equimolar reactions were performed at room temperature, compounds [(M(H(2)dhtp)(H2O)(4)center dot 2H(2)O] (M = Co, Ni) crystallized instead of CPO-27 obtained at the higher temperature of the solvothermal procedure. It was confirmed that mono- and dinuclear species are key building blocks not only in the formation of CPO-27-M but also in the formation of the 1D chain structure (M(H(2)dhtp)(H2O)(4) obtained from these room-temperature reactions.
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