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79959672047
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In this work, we demonstrate that symmetrical bis-salphens can be converted in two steps into bis-salphens with each salphen unit being nonsymmetrical, i.e., a formal desymmetrization in each salphen coordination pocket.
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In this work, we demonstrate that symmetrical bis-salphens can be converted in two steps into bis-salphens with each salphen unit being nonsymmetrical, i.e., a formal desymmetrization in each salphen coordination pocket.
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77957853208
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31
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79959657340
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Note that time may be a decisive parameter as the intermediate species contain imine bonds that are potentially susceptible toward undesired hydrolysis and/or scrambling; this may have affected the overall isolated yield of 12 and 13.
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Note that time may be a decisive parameter as the intermediate species contain imine bonds that are potentially susceptible toward undesired hydrolysis and/or scrambling; this may have affected the overall isolated yield of 12 and 13.
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77956476712
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Anselmo, D.; Escudero-Adán, E. C.; Benet-Buchholz, J.; Kleij, A. W. Dalton Trans. 2010, 39, 8733
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70749149667
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Note that a stepwise templating approach was previously used for the synthesis of nonsymmetrical, heterobimetallic salphens. See
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Note that a stepwise templating approach was previously used for the synthesis of nonsymmetrical, heterobimetallic salphens. See: Castilla, A. M.; Curreli, S.; Martínez Belmonte, M.; Escudero-Adán, E. C.; Benet-Buchholz, J.; Kleij, A. W. Org. Lett. 2009, 11, 5218
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34
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66249123127
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4OAc (see the Supporting Information). The incorporation of OAc donors in these highly Lewis acidic Zn complexes is not surprising taking into account a previous communication from our group. Here we demonstrated that acetate anions may form bridges between two Zn(II) centers, thereby creating supramolecular structures. See:;;, The presence of acetate donors provokes broadening of the NMR signals; the recrystallization of these essentially pure isolated materials was carried out to display sharp NMR patterns to show unequivocally the dissymmetric nature of these compounds.
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4OAc (see the Supporting Information). The incorporation of OAc donors in these highly Lewis acidic Zn complexes is not surprising taking into account a previous communication from our group. Here we demonstrated that acetate anions may form bridges between two Zn(II) centers, thereby creating supramolecular structures. See: Wezenberg, S. J.; Escudero-Adán, E. C.; Benet-Buchholz, J.; Kleij, A. W. Chem.-Eur. J. 2009, 15, 5695 The presence of acetate donors provokes broadening of the NMR signals; the recrystallization of these essentially pure isolated materials was carried out to display sharp NMR patterns to show unequivocally the dissymmetric nature of these compounds.
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Wezenberg, S.J.1
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35
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79959678000
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The LanL2DZ basis set and effective core potential were used for the Zn atoms, and the split-valence 6-31G(d,p) basis set was applied for all other atoms.
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The LanL2DZ basis set and effective core potential were used for the Zn atoms, and the split-valence 6-31G(d,p) basis set was applied for all other atoms.
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36
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79959683879
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The original reactions were performed at 0.012 M, whereas more concentrated reactions were carried out at 0.016, 0.019, and 0.024 M giving isolated yields of 11 in the range 12-35%.
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The original reactions were performed at 0.012 M, whereas more concentrated reactions were carried out at 0.016, 0.019, and 0.024 M giving isolated yields of 11 in the range 12-35%.
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38
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79959683569
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SHELXTL Crystallographic System Ver. 5.10, Bruker AXS, Inc.: Madison, WI.
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Sheldrick, G. M. SHELXTL Crystallographic System Ver. 5.10, Bruker AXS, Inc.: Madison, WI, 1998.
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