Supporting Information

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André Peres
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1 Supporting Information Copper(I)-phosphine polypyridyl complexes: Synthesis, characterization, DA / HSA binding study and antiproliferative activity Wilmer Villarreal a, Legna Colina-Vegas a, Gonzalo Visbal b,c, Oscar Corona d, Rodrigo S. Corrêa a,e, Javier Ellena f, Marcia Regina Cominetti g, Alzir Azevedo Batista a, Maribel avarro *b,h a Departamento de Química, Universidade Federal de São Carlos, CEP , São Carlos-SP, Brazil. b Diretoria de Metrologia Aplicada às Ciências da Vida. Instituto acional de Metrologia, Qualidade e Tecnologia, CEP , Xerém-RJ, Brazil. c Centro de Desenvolvimento em Saúde (CDTS). Fundação Oswaldo Cruz Fiocruz. Rio de Janeiro-RJ, Brazil. d Centro de Química, Instituto Venezolano de Investigaciones Científicas (IVIC), Carretera Panamericana Km.11, Estado Miranda. Apartado Venezuela. e ICEB, Departamento de Química, Universidade Federal de Ouro Preto, CEP , Ouro Preto-MG, Brazil. f Instituto de Física de São Carlos, Universidade de São Paulo, CEP , São Carlos-SP, Brazil. g Departamento de Gerontología, Universidade Federal de São Carlos, CEP , São Carlos-SP, Brazil. h Departamento de Química, Instituto de Ciências Exatas. Universidade Federal de Juiz de Fora, CEP: , Juiz de Fora-MG, Brazil. Fig. S1: Aromatic region of the 1 H-MR spectrum of complex 3 (CDCl 3, 300MHz). Fig. S2: Spectrophotometric titration spectra of copper complexes 1-5 with CT-DA. Fig. S3: Spectrofluorometric titration spectra of HSA with the copper compounds 1-5. Fig. S4: Distribution coefficients of copper complexes in a 1:1 n-octanol buffer mixture. Fig. S5: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (phen)]o 3 at different times. Fig. S6: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dpq)]o 3 at different times. Fig. S7: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dppz)]o 3 at different times. Fig. S8: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dppa)]o 3 at different times. Fig. S9: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dppme)]o 3 at different times. Table S1: X-Ray crystallographic data collection and refinement parameters for complex 3.

2 Figure S1: Aromatic region of the 1 H-MR spectrum of complex 3 (CDCl 3, 300MHz). c a d e b P P Cu + c b a d e c a d e b c a d e b P P Cu + c b a d e

3 Figure S2: Spectrophotometric titration spectra of copper complexes 1-5 with CT- DA.

4 Figure S3: Spectrofluorometric titration spectra of HSA with the copper compounds 1-5.

5 Figure S4: Distribution coefficients of copper complexes in a 1:1 n-octanol buffer mixture

6 Absorbance Wavelength (nm) 0 h 12 h 24 h 48 h Cuphen Figure S5: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (phen)]o 3 at different times.

7 Absorbance Wavelength (nm) 0 h 12 h 24 h 48 h Cudpq Figure S6: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dpq)]o 3 at different times.

8 Absorbance Wavelength (nm) 0 h 12 h 24 h 48 h Cudppz Figure S7: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dppz)]o 3 at different times.

9 Absorbance Wavelength (nm) 0 h 12 h 24 h 48 h Cudppa Figure S8: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dppa)]o 3 at different times.

10 Absorbance Wavelength (nm) 0 h 12 h 24 h 48 h Cudppme Figure S9: 1 H and 31 P{ 1 H} MR spectrum in DMSO-d 6 (upper panel) and UV-Vis spectra in DMSO (lower panel) of complex [Cu(PPh 3 ) 2 (dppme)]o 3 at different times.

11 Table S1. X-Ray crystallographic data collection and refinement parameters for complex 3. Empirical formula Formula weight Temperature Wavelength Crystal system Space group P-1 [CuC 54 H 40 4 P 2 ]. O 3.CH 3 OH 293(2) K Å triclinic Unit cell dimensions a = (5) Å α= (5). b = (5) Å β= (5). c = (5) Å γ = (5). Volume (15) Å 3 Z 2 Density (calculated) Mg/m 3 Absorption coefficient F(000) mm-1 Crystal size 0.30 x 0.15 x 0.8 mm 3 Theta range for data collection 2.95 to Index ranges Reflections collected h 13, -18 k 18, -20 l 20 Independent reflections 9735 [R(int) = ] Completeness to theta = % Refinement method Full-matrix least-squares on F 2 Data / restraints / parameters 9735 / 0 / 605 Goodness-of-fit on F Final R indices [I>2sigma(I)] R1 = , wr2 = R indices (all data) R1 = , wr2 = Extinction coefficient 0.030(3) Largest diff. peak and hole and e.å -3

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