Electronic supplementary information (ESI) Multinuclear Ni ... · Electronic supplementary information (ESI) Multinuclear Ni(II), Cu(II) and Zn(II) complexes of chiral macrocyclic
This document is posted to help you gain knowledge. Please leave a comment to let me know what you think about it! Share it to your friends and learn new things together.
Transcript
Electronic supplementary information (ESI)
Multinuclear Ni(II), Cu(II) and Zn(II) complexes of chiral macrocyclic nonaazamine
Marta Löffler*, Janusz Gregoliński, Maria Korabik, Tadeusz Lis and Jerzy Lisowski
Faculty of Chemistry, University of Wrocław, 14 F. Joliot-Curie, 50-383, Wrocław, Poland. E-mail: [email protected]
Supporting Figure 1S. The CD spectra of the two enantiomeric complexes [Ni3(L)(H2O)2Cl5]Cl in methanol (C = 1∙10-3 M ): [Ni3(R-L)(H2O)2Cl5]Cl (red)/ [Ni3(S-L)(H2O)2Cl5]Cl (blue).
Supporting Figure 2S.The CD spectra of the two enantiomeric complexes [Cu3( L)Cl4]Cl2 in methanol (C = 1∙10-3 M): [Cu3(R- L)Cl4]Cl2 (red)/ [Cu3(S- L)Cl4]Cl2 (blue).
3
Supporting Figure 3S.The CD spectra of the two enantiomeric complexes [Zn2(L)Cl2](ZnCl4) in methanol (C = 1∙10-3 M): [Zn2(R-L)Cl2](ZnCl4) (red)/ [Zn2(S-L)Cl2](ZnCl4) (blue).
NMR spectra
Supporting Figure S4. 1H NMR spectrum (500 MHz) of [Ni3(R-L)(H2O)2Cl5]Cl in CD3CN solution.
4
Supporting Figure 5S. VT-1H NMR spectra (500 MHz) of [Ni3(R-L)(H2O)2Cl5]Cl in CD3CN solution.
Supporting Figure 6S. 1H NMR spectrum (500 MHz) of [Cu3(R- L)Cl4]Cl2 in D2O solution.
5
Supporting Figure 7S. VT- 1H NMR spectra (300 MHz) of [Cu3(R- L)Cl4]Cl2 in D2O solution.
Supporting Figure 8S. 1H NMR spectrum (500 MHz) of [Zn2(R-L)Cl2](ZnCl4) in CDCl3/CD3OD (v/v 2/1) solution.
Supporting Figure 13S. Fragment of HMQC spectrum (500 MHz, CDCl3/CD3OD v/v 2/1 solution) of [Zn2(R-L)Cl2](ZnCl4) complex.
Supporting Figure 14S. Fragment of HMQC spectrum (500 MHz, CDCl3/CD3OD v/v 2/1 solution) of [Zn2(R-L)Cl2](ZnCl4) complex.
9
Supporting Figure 15S. Fragments of 1H NMR spectra (500 MHz) received during the titration of R-L ligand with ZnCl2 in CDCl3/CD3OD solution. Bottom - spectrum of R-L ligand, top - spectrum of [Zn2(R-L)Cl2](ZnCl4) complex. Asterisk denotes the residual solvent signal.
10
Supporting Figure 16S. 1H NMR spectra (500 MHz) received during the titration of R-L ligand with ZnCl2 in CDCl3/CD3OD solution.
Supporting Figure 17S. The comparison of macrocyle conformation and metal ion positions in protonated R-L and trinuclear complexes [Cu3(R- L)(-OH)2]Cl2(ClO4)2, [Cu3(R- L)Cl4]Cl2, [Ni3(R-L)(H2O)2Cl5]Cl, and [Zn2(R-L)Cl2](ZnCl4), respectively.
13
Supporting Figure 18S. Very week intermolecular H-bonds for complex [Ni3(R-L)(H2O)2Cl5]Cl·0.4CH3CN·4.2H2O between nitrogen atom of macrocyclic ligand and terminal chloride atom [N8∙∙∙Cl3` 3.696 Å; N8-H8∙∙∙Cl3` 169.6°; -x+1, y-1/2, -z+3/2 ] which forms 1D zig-zag polymer. The shortest intermolecular distance between two nickel atoms of adjacent molecules is equal to 6.709(6) Å for Ni3-Ni1`.
Supporting Figure 19S. Intermolecular H-bonds for complex [Cu3(R-L)Cl4]Cl2·CH3CN·7.5(H2O) between nitrogen atoms of macrocyclic ligand and chloride atoms [N2∙∙∙Cl4` 3.215 Å; N2-H2∙∙∙Cl4` 169.13°; -x+3/2, -y+1, z+1/2 and N8∙∙∙Cl2` 3.499 Å; N8-H8∙∙∙Cl2` 163.19°; -x+3/2, -y+1, z+1/2] which forms 1D polymer. The shortest intermolecular distance between two copper atoms of adjacent molecules is equal to 5.846(4) Å for Cu1-Cu3`[x+3/2, -y+1, z+1/2 ].
14
MS spectra
Supporting Figure 20S. ESI MS spectra of [Ni3(R-L)(H2O)2Cl5]Cl.
Supporting Figure 21S. ESI MS spectra of [Cu3(R- L)Cl4]Cl2.
15
Supporting Figure 22S. ESI MS spectra of [Zn2(R-L)Cl2](ZnCl4).