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34547949856
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note
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f = 0.05%).
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76
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16244375491
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note
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1H NMR chemical shift behavior. Regardless, they are a minor component in the equilibria when compared to the stabilities of the prevailing 1:1 complexes.
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77
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16244415150
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note
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v = 15 321/967 with I > 2σ(I). All of the non-hydrogen atoms were refined with anisotropic thermal parameters. The hydrogen atom positions were calculated geometrically and were included as riding on their respective carbon atoms. CCDC 253083 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/ data_request/cif.
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78
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16244396377
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note
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v = 7071/457 with I > 2σ(I). All of the non-hydrogen atoms were refined with anisotropic thermal parameters. The hydrogen atom positions were calculated geometrically and were included as riding on their respective carbon atoms. CCDC 253084 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from the Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.
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79
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16244392682
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The least-squares plane of the macrocycle was calculated using the four carbonyl carbon atoms. Calculation of the angle between the Cl-Pd-Cl axis and the plane that bisects the isophthalamide aryl ring was performed by calculating the angle between the planes perpendicular to the lines defined by a) the Cl-Pd-Cl axis and b) the line described by the two carbonyl-substituted carbon atoms of the isophthalamide ring. The value obtained had 90° subtracted from it to arrive at the final figure.
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16244376416
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We very recently confirmed the synthesis of a [2]rotaxane by this method in our laboratories, the results of which will be reported in due course.
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