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

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DOIResolve DOI: http://doi.org/10.1080/1061027031000139349
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TypeArticle
Journal titleSupramolecular Chemistry
Volume15
Issue6
Pages433-446(14)
AbstractVarious 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 <PRE>13</PRE>C 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 isostructural TATM inclusion compounds. Only 1,9-dichlorononane and 1,10-dichlorodecane form isostructural TATM inclusion compounds. This behaviour is compared with isostructuralism among previously studied TATM-alkyl halide guest systems. DSC experiments were performed to determine the relationship between the size of guest and the thermal properties of the inclusion compound. We found a direct relationship between the melting temperature and the heat of fusion. These data are compared to a recent study on urea-carboxylic acid complexes.
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AffiliationNational Research Council Canada; NRC Steacie Institute for Molecular Sciences
Peer reviewedNo
NPARC number12328339
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Record identifierbc5d0294-7fdb-4d48-9b5b-40d60df5a41d
Record created2009-09-10
Record modified2016-05-09
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