flexible, linear, tetranuclear palladium complexes supported ...flexible, linear, tetranuclear...

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T. Tanase et al. Electronic Supplementary Information S-1 Electronic Supplementary Information (ESI) for Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups Tomoaki Tanase,* Satoko Hatada, Ayaka Mochizuki, Kanako Nakamae, Bunsho Kure and Takayuki Nakajima Department of Chemistry, Faculty of Science, Nara Women’s University, Kitauoya-nishi-machi, Nara 630-8506, Japan E-mail: [email protected] Fig. S1. 31 P{ 1 H} NMR spectrum of dpmppmF 2 in CDCl 3 (b) with a simulated spectrum (a). Fig. S2 31 P{ 1 H} NMR spectrum of 5 in CD 2 Cl 2 at room temperature. Fig. S3. Variabletemperature UVvis absorption spectra of 6 in CH 2 Cl 2 . Fig. S4. Variabletemperature UVvis absorption spectra of 3 in CH 2 Cl 2 . Fig. S5. 19 F NMR spectra for the dpmppmF 2 region of 1 at 80 ºC in CD 2 Cl 2 (a) and at 60 ºC in CD 3 CN (b). Fig. S6. Temperaturedependent (a) 31 P{ 1 H}, (b) 1 H and (c) 19 F NMR spectra of 2 in CD 2 Cl 2 (80ºC < T < 20 ºC). Fig. S7. Temperaturedependent (a) 31 P{ 1 H}, (b) 1 H and (c) 19 F NMR spectra of 4 in CD 2 Cl 2 (80ºC < T < 20 ºC) Fig. S8. Temperaturedependent (a) 31 P{ 1 H}, (b) 1 H and (c) 19 F NMR spectra of 3 in CD 2 Cl 2 (80ºC < T < 20 ºC) Fig. S9 DFT optimized structures of (a) [Pd 4 (dpmppmF 2 ) 2 (XylNC) 3 ] 2+ (1) and (b) [Pd 4 (dpmppmF 2 ) 2 (XylNC) 2 ] 2+ (1) with selected structural parameters. DFT calculations were performed with B3LYP/lanl2dz methods. Fig. S10 Values of natural charge (red) and Wiberg bond indices (blue) derived from Natural Bond Analyses on the DFT optimized structures of (a) [Pd 4 (dpmppmF 2 ) 2 (XylNC) 3 ] 2+ (1) and (b) [Pd 4 (dpmppmF 2 ) 2 (XylNC) 2 ] 2+ (1). Electronic Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2013

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Page 1: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-1

Electronic Supplementary Information (ESI)

for

Flexible, linear, tetranuclear palladium complexes supported by

tetraphosphine ligands with electron-withdrawing groups

Tomoaki Tanase,* Satoko Hatada, Ayaka Mochizuki, Kanako Nakamae, Bunsho Kure and

Takayuki Nakajima

Department of Chemistry, Faculty of Science, Nara Women’s University,

Kitauoya-nishi-machi, Nara 630-8506, Japan

E-mail: [email protected]

Fig. S1. 31

P{1H} NMR spectrum of dpmppmF2 in CDCl3 (b) with a simulated spectrum (a).

Fig. S2 31

P{1H} NMR spectrum of 5 in CD2Cl2 at room temperature.

Fig. S3. Variabletemperature UVvis absorption spectra of 6 in CH2Cl2.

Fig. S4. Variabletemperature UVvis absorption spectra of 3 in CH2Cl2.

Fig. S5. 19

F NMR spectra for the dpmppmF2 region of 1 at 80 ºC in CD2Cl2 (a) and at 60 ºC in CD3CN (b).

Fig. S6. Temperaturedependent (a) 31

P{1H}, (b)

1H and (c)

19F NMR spectra of 2 in CD2Cl2 (80ºC < T < 20 ºC).

Fig. S7. Temperaturedependent (a) 31

P{1H}, (b)

1H and (c)

19F NMR spectra of 4 in CD2Cl2 (80ºC < T < 20 ºC)

Fig. S8. Temperaturedependent (a) 31

P{1H}, (b)

1H and (c)

19F NMR spectra of 3 in CD2Cl2 (80ºC < T < 20 ºC)

Fig. S9 DFT optimized structures of (a) [Pd4(dpmppmF2)2(XylNC)3]2+

(1) and (b)

[Pd4(dpmppmF2)2(XylNC)2]2+

(1’) with selected structural parameters. DFT calculations were performed with

B3LYP/lanl2dz methods.

Fig. S10 Values of natural charge (red) and Wiberg bond indices (blue) derived from Natural Bond Analyses on the

DFT optimized structures of (a) [Pd4(dpmppmF2)2(XylNC)3]2+

(1) and (b) [Pd4(dpmppmF2)2(XylNC)2]2+

(1’).

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013

Page 2: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-2

Fig. S1. 31

P{1H} NMR spectrum of dpmppmF2 in CDCl3 (b) with a simulated spectrum (a).

Fig. S2 31

P{1H} NMR spectrum of 5 in CD2Cl2 at room temperature.

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013

Page 3: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-3

Fig. S3. Variabletemperature UVvis absorption spectra of 6 in CH2Cl2.

Fig. S4. Variabletemperature UVvis absorption spectra of 3 in CH2Cl2.

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013

Page 4: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-4

Fig. S5. 19

F NMR spectra for the dpmppmF2 region of 1 at 80 ºC in CD2Cl2 (a) and at 60 ºC in

CD3CN (b).

Fig. S6. Temperaturedependent (a) 31

P{1H}, (b)

1H and (c)

19F NMR spectra of 2 in CD2Cl2

(80ºC < T < 20 ºC). The asterisks indicate impurity.

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013

Page 5: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-5

Fig. S7. Temperaturedependent (a) 31

P{1H}, (b)

1H and (c)

19F NMR spectra of 4 in CD2Cl2

(80ºC < T < 20 ºC). The asterisks indicate impurity.

Fig. S8. Temperaturedependent (a) 31

P{1H}, (b)

1H and (c)

19F NMR spectra of 3 in CD2Cl2

(80ºC < T < 20 ºC). The asterisks indicate impurity.

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013

Page 6: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-6

Fig. S9 DFT optimized structures of (a) [Pd4(dpmppmF2)2(XylNC)3]2+

(1) and (b)

[Pd4(dpmppmF2)2(Xyl-NC)2]2+

(1’) with selected structural parameters. DFT calculations were

performed with B3LYP/lanl2dz methods.

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013

Page 7: Flexible, linear, tetranuclear palladium complexes supported ...Flexible, linear, tetranuclear palladium complexes supported by tetraphosphine ligands with electron-withdrawing groups

T. Tanase et al.

Electronic Supplementary Information

S-7

Fig. S10 Values of natural charge (red) and Wiberg bond indices (blue) derived from Natural

Bond Analyses on the DFT optimized structures of (a) [Pd4(dpmppmF2)2(XylNC)3]2+

(1) and

(b) [Pd4(dpmppmF2)2(XylNC)2]2+

(1’).

Electronic Supplementary Material (ESI) for Dalton TransactionsThis journal is © The Royal Society of Chemistry 2013