Solvent-drop assisted mechanochemical synthesis of the black and green polymorphs of the tetrathiafulvalene–chloranil charge transfer salt |
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Authors: | Shermane Benjamin Silvina Pagola Zachary Huba Everett Carpenter Tarek Abdel-Fattah |
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Affiliation: | 1. Rowan University, 201 Mullica Hill Rd., Glassboro, NJ 08028, USA;2. Applied Research Center, 12050 Jefferson Avenue, Newport News, VA, 23606, USA, and College of William and Mary, Department of Applied Science, McGlothlin-Street Hall 314, Williamsburg, VA, 23185, USA;3. Department of Chemistry, Virginia Commonwealth University, 1001 West Main St., Richmond, VA 23284, USA;4. Applied Research Center, 12050 Jefferson Avenue, Newport News, VA, 23606, USA, and Department of Biology, Chemistry and Environmental Science, Christopher Newport University, Newport News, VA, 23606, USA |
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Abstract: | This work describes the synthesis of the green and black polymorphic forms of the tetrathiafulvalene–chloranil (TTF–CA) charge transfer salt as pure phases, by solvent-assisted mechanochemistry. Both materials were characterized using laboratory and high-resolution X-ray powder diffraction (XRPD), elemental analysis and scanning electron microscopy (SEM). The high-resolution XRPD pattern of the TTF–CA black polymorph was indexed with a triclinic lattice a = 10.756(5) Å, b = 11.057(4) Å, c = 6.614(2) Å, α = 101.36(2)°, β = 93.69(3)°, γ = 89.37(3)°, V = 769.6(5) Å3. The chemical stability of these phases upon heating was investigated using thermogravimetric analysis (TGA), elemental analysis and X-ray powder diffraction (XRPD), indicating that both polymorphs undergo chemical decomposition, and ruling out the transition to an air-stable high temperature polymorph. |
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