Eur. J. Inorg. Chem WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim, 2006 ISSN SUPPORTING INFORMATION

Transcription

1 Eur. J. Inorg. Chem WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim, 2006 ISSN SUPPORTING INFORMATION Title: Synthesis, Structures and Catecholase Activity of a New Series of Dicopper(II) Complexes of Reduced Schiff Base Ligands Author(s): Bellam Sreenivasulu, Fei Zhao, Song Gao, Jagadese J. Vittal* Ref. No.: I

2 Table S1 ESI-MS data for 1-13 Complex Solvent Principal molecular species (m/z), % peak height) a [Cu 2 (Scp11) 2 (H 2 O) 2 ], 1 MeOH [Cu 2 (Scp11) 2 H] + ( ) [Cu 2 (Scp11) 2 Na] + (614, 80); [Cu 3 (Scp11) 3 Na] + (912, 52); [Cu 4 (Scp11) 4 H] + (1188.8, 25); [Cu 4 (Scp11) 4 Na] + (1208, 80); [Cu 5 (Scp11) 5 Na + ] (1504, 40); [Cu 6 (Scp11) 6 Na + ] (1803.5, 30) [Cu 2 (ClScp11) 2 (H 2 O) 2 ], 2 MeOH/ DMSO [Cu 2 (ClScp11) 2 H] + (699, 100) [Cu(ClScp11) 2 (DMSO)Na] + (699.1, 50); [Cu 2 (ClScp11) 2 (DMSO)H] + (818.4, 20); [Cu 3 (ClScp11) 3 (DMSO)H] + (1152.7, 22); [Cu 4 (ClScp11) 3 (DMSO) 4 ] + (1370.7, 52); [Cu 2 (MeScp11) 2 (H 2 O) 2 ], 3 MeOH [Cu 2 (MeScp11) 2 (CH 3 OH)Na] + (678.9, 100); [Cu 2 (MeScp11) 2 (CH 3 OH)H] + (654.9, 28); [Cu 2 (MeScp11) 3 ] - (870.1, 20); [Cu 3 (MeScp11) 4 ] - (1179.9, 28); [Cu 4 (MeScp11) 5 ] - (1492.0, 30)

3 [Cu 2 (OHScp11) 2 ].(H 2 O) 2 ], 4 MeOH [Cu 2 (OHScp11) 2 ] - (623.1, 100); [Cu(OHScp11) 2 ] - (562.2, 85); [Cu(OHScp11)] - (311.0, 44); [Cu 2 (OHScp11) 3 ] - (874.3, 50); [Cu 3 (OHScp11) 3 ] - (937.4, 30) [Cu 2 (Sch11) 2 ].(H 2 O), 5 MeOH [Cu 2 (Sch11) 3 ] - (868.2, 100); [Cu 3 (Sch11) 4 ] - (1180.2, 21); [Cu 4 (Sch11) 5 ] - (1490.0, 30); [Cu 2 (ClSch11) 2 (H 2 O) 2 ], 6 MeOH [Cu 2 (ClSch11) 2 H] + (726.1, 100) [Cu 2 (ClSch11) 3 ] - (972.4, 75); [Cu(ClSch11) 2 ] - (628, 40) [Cu 2 (MeSch11) 2 (H 2 O) 2 ], 7 MeOH/ DMSO [Cu 2 (MeSch11)] + (388.9, 100); [Cu 2 (MeSch11) (DMSO)] + (466.5, 75); [Cu 2 (MeSch11) 2 H] + (649, 25); [{Cu 2 (Sch12) 2 } 2 Cu 2 (Sch12) 2 (H 2 O) 2 ].4H 2 O, 8 MeOH [Cu 2 (Sch12) 2 Na] + (643.0, 100); [Cu(Sch12)Na] + (333.0, 27); [Cu 3 (Sch12) 3 Na] + (954.9, 55); [Cu 4 (Sch12) 4 Na] + (1267.7, 25); [Cu 5 (Sch12) 5 Na] + (1574.5, 20) MeOH/ DMSO [Cu 2 (ClSch12) 3 (DMSO)] - (1051.0, 100); [Cu(ClSch12) 2 ] - (627.1, 11); [Cu 2 (ClSch12) 3 ] - (973, 23); [Cu 3 (ClSch12) 4 ] - (1318.0, 28) [Cu 2 (MeSch12) 2 (H 2 O) 2 ], 10 MeOH [Cu 2 (MeSch12) 2 (CH 3 OH)H] + [Cu 2 (ClSch12) 2 (H 2 O) 2 ], 9 (680.0, 100); [Cu(MeSch12)H] + (325.1, 20); [Cu 3 (MeSch12) 2 ] + (709.2, 50) [Cu 2 (H 3 Diala5) 2 (H 2 O) 2 ].H 2 O, 11 MeOH [Cu 3 (Diala5) 3 H] + (817.0, 100) [Cu(Diala5)H] + (272.2, 25); [Cu 4 (Diala5) 4 H] + (1090.9, 60); [Cu 5 (Diala5) 5 H] + (1364, 40); [Cu 6 (Diala5) 6 H] + (1634.6, 40); [Cu 7 (Diala5) 7 H] + (1908.6, 30) [Cu 2 (H 3 Diala4) 2 (H 2 O) 2 ].H 2 O, 12 MeOH [Cu 2 (Diala4) 2 Na] + (566.9, 100); [Cu 2 (Diala4) 2 H] + (544.7, 40); [Cu 3 (Diala4) 3 Na] + (840.8, 78); [Cu 4 (Diala4) 2 Na] + (1090.7, 50); [Cu 5 (Diala4) 5 Na] + (1386.5, 60); [Cu 6 (Diala4) 6 Na] + (1658.5, 22) [Cu 2 (H 3 Diala3 ) 2 (H 2 O) 2 ].H 2 O, 13 MeOH [Cu 2 (Diala3 ) 2 Na] + (577.2, 100) [Cu 2 (Diala3 ) 2 H] + (544.8, 40); [Cu(Diala3 )H] + (272.9, 35); [Cu 3 (Diala3 ) 3 H] + (818.7, 30); [Cu 4 (Diala3 ) 4 H] + (1090.6, 22)

4 a. Percentage refers to the height relative to the most intense peak in the spectrum Figure S1. ESI-mass spectrum of 8 Figure S2. A perspective view of the unit cell contents of 2a

5 Figure S3. Hydrogen bonded association in 2a Figure S4. A perspective view of 3a (Symmetry equivalent positions: -x+1,-y+1,-z+1)

6 Figure S5. Packing diagram of 3a Figure S6. A perspective view of 6a (Symmetry equivalent postions: -x+1,-y+1,-z+1)

7 Figure S7. Packing diagram of 6a Figure S8. A view of the unit cell contents of 9a

8 Figure S9. A portion of the 1D structure formed between 9 and methanol molecules 9a Figure S10. Perspective view of 12a

9 Figure S11. Packing pattern in 12a Figure S12. TGA and DTG of complex 1

10 Figure S13. TGA and DTG of complex 2 Figure S14. TGA and DTG of complex 3

11 Figure S15. TGA and DTG of complex 4 Figure S16. TGA and DTG of complex 5

12 Figure S17. TGA and DTG of complex 6 Figure S18. TGA and DTG of complex 7

13 Figure S19. TGA and DTG of complex 8 Figure S20. TGA and DTG of complex 9

14 Figure S21. TGA and DTG of complex 10 Figure S22. TGA and DTG of complex 11

15 Figure S23. TGA and DTG of complex 12 Figure S24. TGA and DTG of complex 13

16 Figure S25. UV-Vis plots of the oxidation of 3,5-DTBC by 1 Figure S26. Lineweaver-Burk plot for 1

17 Figure S27. UV-Vis plots of the oxidation of 3,5-DTBC by 2 Figure S28. Lineweaver-Burk plot for 2

18 Figure S29. UV-Vis plots of the oxidation of 3,5-DTBC by 3 Figure S30. Lineweaver-Burk plot for 3

19 Figure S31. UV-Vis plots of the oxidation of 3,5-DTBC by 4 Figure S32. Lineweaver-Burk plot for 4

20 Figure S33. UV-Vis plots of the oxidation of 3,5-DTBC by 5 Figure S34. Lineweaver-Burk plot for 5

21 Figure S35. UV-Vis plots of the oxidation of 3,5-DTBC by 6 Figure S36. Lineweaver-Burk plot for 6

22 Figure S37. UV-Vis plots of the oxidation of 3,5-DTBC by 7 Figure S38. Lineweaver-Burk plot for 7

23 Figure S39. UV-Vis plots of the oxidation of 3,5-DTBC by 9 Figure S40. Lineweaver-Burk plot for 9

24 Figure 41. UV-Vis plots of the oxidation of 3,5-DTBC by 10 Figure 42. Lineweaver-Burk plot for 10

25 Figure 43. UV-Vis plots of the oxidation of 3,5-DTBC by 11 Figure S44. Lineweaver-Burk plot for 11

26 Figure S45. UV-Vis plots of the oxidation of 3,5-DTBC by 12 Figure S46. Lineweaver-Burk plot for 12

27 Figure S47. UV-Vis plots for the oxidation of 3,5-DTBC by 13 Figure S48. Lineweaver-Burk plot for 13

28 Figure S49. Typical plot for Absorption Vs Time during kinetic studies. Curve a at the starting concentration of the substrate (1.0x10-3 M) and curve e at the final concentration of the substrate (1.3x10-2 M).