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13C NMR, and IR spectroscopy; EI, FAB, or MALDI-TOF mass spectrometry; and elemental analysis or high-resolution mass spectrometry. The rods 4a/4b and 19a/19b were additionally characterized by UV/VIS and fluorescence spectroscopy.
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2O resonances were evaluated. In the fluorescence titrations at constant concentration of the molecular rod (c(rod) ≈ 0.01-0.02 mM, c(dendrophane) = 0.005-0.8 mM), the emission intensity of the rod decreased upon addition of dendrophane and the emission maxima of 4a/4b at saturation binding shifted by 5-16 nm to higher energy.
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3(19) of the steroids in solutions of 4a and 2 are compatible with formation of a 2:1 complex; that is, they are of similar magnitude to those observed for these resonances in the 1:1 complexes formed by testosterone (11) or the mono-steroid rods 18a and 18b.
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0344695061
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1H NMR titrations to determine stabilities of the complexes formed by 4b.
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