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In the first series of experiments, the spectrum of 1 recorded in the presence of commercially available CB7 (Aldrich, showed additional signals in addition to those attributable to the free and included species that were erroneously assigned to the nitroxide included in CB7 from the benzyl side on the basis of the a(N) values. However, repetition of the EPR experiments with new batches of commercial CB7 resulted in the formation of only one included species that was attributed to the nitroxide included from a single side see text, Analogous results were obtained with CB7 synthesised in our laboratory. We suppose that traces of some impurities present in the first batch of commercial CB7 employed were responsible for the formation of a different type of complex
-
In the first series of experiments, the spectrum of 1 recorded in the presence of commercially available CB7 (Aldrich). showed additional signals in addition to those attributable to the free and included species that were erroneously assigned to the nitroxide included in CB7 from the benzyl side on the basis of the a(N) values. However, repetition of the EPR experiments with new batches of commercial CB7 resulted in the formation of only one included species that was attributed to the nitroxide included from a single side (see text). Analogous results were obtained with CB7 synthesised in our laboratory. We suppose that traces of some impurities present in the first batch of commercial CB7 employed were responsible for the formation of a different type of complex.
-
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104
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0002798427
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For examples, see: a
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Recent review on the effect of solvent in determining the hyperfine coupling constants of free radicals
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[1]
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34548362602
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1H NMR spectrum of CB7@4 does not shown any differentiation of the host's methylene protons of the portals, reflecting the different nature of the complex in which the TEMPO radical is inserted in a symmetrical fashion with the NO group lying on the plane passing through the equatorial carbon-carbon bonds of the host.
-
1H NMR spectrum of CB7@4 does not shown any differentiation of the host's methylene protons of the portals, reflecting the different nature of the complex in which the TEMPO radical is inserted in a symmetrical fashion with the NO group lying on the plane passing through the equatorial carbon-carbon bonds of the host.
-
-
-
-
111
-
-
34548318054
-
-
[5l] respectively.
-
[5l] respectively.
-
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114
-
-
34548322232
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Unfortunately, we failed to obtain a suitable crystal of the CB7@2 complex for X-ray analysis.
-
Unfortunately, we failed to obtain a suitable crystal of the CB7@2 complex for X-ray analysis.
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34548337796
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Because the concentration of the added host and salt is comparable to that of the probe in most cases, the free concentrations of the components were calculated by solving the mass balance equations by means of the Newton-Raphson method.[35
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[35]
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34548359857
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Radical 1 shows an unexpected low persistence in the presence of CB7 at temperatures higher than 40°C. For this reason, an accurate determination of the activation parameters for the coordination process was not possible.
-
Radical 1 shows an unexpected low persistence in the presence of CB7 at temperatures higher than 40°C. For this reason, an accurate determination of the activation parameters for the coordination process was not possible.
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125
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34548307785
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Similar solution-phase ternary complexes having calixarenes as macrocyclic hosts have been recently reported: H. Bakirci, A. L. Koner, M. H. Dickman, U. Kortz, W. M. Nau, Angew. Chem. 2006, 118, 7560-7564;
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Similar solution-phase ternary complexes having calixarenes as macrocyclic hosts have been recently reported: H. Bakirci, A. L. Koner, M. H. Dickman, U. Kortz, W. M. Nau, Angew. Chem. 2006, 118, 7560-7564;
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