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Nine new cobalt fluorophosphates frameworks have been synthesised hydrothermally in a fluoride-rich medium, through the use of CoF3 and HPF6 as reactants in combination with Group I/II metal hydroxides and organic cations as templating species. Products have been structurally characterised using single crystal X-ray diffraction. Reaction in fluoride-rich conditions produces chain, layer and three dimensional framework structures containing new and unusual structural features based on the linking of PO3F, PO2(OH,F)2 and Co(O,F)n polyhedra (n = 5–6) including μ2, μ3 and μ4 bridging fluoride. Structures exhibiting inter-layer spaces and channels frequently have these lined by terminal fluoride anions of the PO3F, PO2(OH,F)2 and Co(O,F)n polyhedra.
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