Physicochemical Characterization of Tris(5-acetyl-3-thienyl)methane Inclusion Compounds with 1,n-Dichloroalkane Guests (n=1 to 10). A Combined TGA, 13C CP/MAS NMR, Powder X-ray Diffraction and DSC Study

2003 
Various physicochemical characterization techniques were used to study tris(5-acetyl-3-thienyl)methane (TATM) inclusion compounds with 1,n-dichloroalkane guests (n = 1 -- 10). Thermogravimetric analysis (TGA) experiments allowed us to determine host–guest stoichiometric ratios. We determined that the smallest size guests (n = 1 -- 4) form 2H:1G TATM inclusion compounds, the intermediate size guests (n=5 and 6) form 3H:1G TATM inclusion compounds, while the largest size guests (n = 8 -- 10) form 4H:1G TATM inclusion compounds. From the multiplicity of the host signals in the 13C CP/MAS NMR spectrum, we were able to determine the number of host molecules in the asymmetric unit of each inclusion compound. For n = 1 -- 4, there is 1 TATM molecule in the asymmetric unit, for n=5 and 6, there are 3 TATM molecules in the asymmetric unit, while for n = 8 -- 10, there are 2 TATM molecules in the asymmetric unit. Powder X-ray diffraction experiments were conducted to determine if any of the nine guests form isostru...
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