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1 Electronic Supplementary Material (ESI) for Dalton Transactions. This journal is The Royal Society of Chemistry 2014 Electronic Supporting Information Assembly of HeterobimetallicNi II -Ln III (Ln III = Dy III, Tb III, Gd III,Ho III, Er III, Y III ) Complexes Using a Ferrocene Ligand: Slow Relaxation of the Magnetization in Dy III, Tb III and Ho III Analogues AmitChakraborty, a PrasenjitBag, a Eric Rivière, b TalalMallah b, VadapalliChandrasekhar a,c a Department of Chemistry, Indian Institute of Technology Kanpur, Kanpur , India b Institut de ChimieMoleculaire et Mate riaux d'rsay, Universite Paris-Sud 11, F-91405, rsay, France c National Institute of Science Education and Research, Institute of Physics Campus, SachivalayaMarg, Sainik School Road, Bhubaneshwar , disha, India. S1
2 Table S1. Bond lengths around Bond angles around Terbium(III) Terbium(III) Fe N 1 N 3 N 2 N 4 13 H 2 Ni Tb N 5 9 (Å) Tb(1)-(6) 2.304(5) Tb(1)-(3) 2.320(5) ( ) (3)-Tb(1)-(1) 70.05(18) (3)-Tb(1)-(4) 63.70(18) N 6 12 Tb(1)-(1) 2.331(5) (1)-Tb(1)-(2) 62.49(17) Tb(1)-(8) 2.423(6) (4)-Tb(1)-(2) (19) Tb(1)-(7) 2.460(7) Tb(1)-(11) 2.467(6) Bond angles around Tb(1)-(10) 2.499(6) Nickel(II) Tb(1)-(4) 2.529(6) ( ) Tb(1)-(2) 2.613(6) Bond lengths (3)-Ni(1)-(1) 81.5(2) around Nickel(II) (1)-Ni(1)-N(2) 87.3(2) (Å) (3)-Ni(1)-N(4) 87.0(2) Ni(1)-(5) 2.017(5) Ni(1)-(3) 2.036(5) Ni(1)-(1) 2.055(5) N(2)-Ni(1)-N(4) 104.2(2) Ni(1)-(1)-Tb(1) 102.5(2) Ni(1)-(3)-Tb(1) 103.5(2) Ni(1)-N(2) 2.076(6) Ni(1)-(13) 2.091(6) Ni(1)-N(4) 2.126(6) S2
3 Table S2. Bond lengths around Bond angles around Holmium(III) Holmium(III) N 1 N 2 13 H N 5 9 (Å) ( ) Fe N 3 N 4 Ni Ho N 6 1 Ho(1)-(6) 2.284(3) Ho(1)-(3) 2.296(2) Ho(1)-(1) 2.307(3) Ho(1)-(8) 2.407(3) Ho(1)-(10) 2.438(3) Ho(1)-(7) 2.451(3) Ho(1)-(11) 2.485(3) Ho(1)-(4) 2.534(3) (3)-Ho(1)-(1) 70.43(9) (3)-Ho(1)-(4) 63.97(9) (1)-Ho(1)-(2) 62.86(8) (4)-Ho(1)-(2) (9) Bond angles around Nickel(II) ( ) Ho(1)-(2) 2.610(3) (3)-Ni(1)-(1) 80.89(10) (1)-Ni(1)-N(2) 87.84(11) Bond lengths around Nickel(II) (Å) (3)-Ni(1)-N(4) 87.24(11) N(2)-Ni(1)-N(4) (11) Ni(1)-(1)-Ho(1) (11) Ni(1)-(3)-Ho(1)103.49(11) Ni(1)-(5) 2.023(3) Ni(1)-(3) 2.038(3) Ni(1)-(1) 2.054(2) Ni(1)-N(2) 2.073(3) Ni(1)-(13) 2.098(3) S3
4 Ni(1)-N(4) 2.130(3) Table S3. Bond lengths around Bond angles around Gadolinium(III) Gadolinium(III) N 1 N 2 13 H N 5 9 (Å) ( ) Fe N 3 N 4 Ni Gd N 6 12 Gd(1)-(6) 2.325(4) Gd(1)-(1) 2.331(4) Gd(1)-(3) 2.350(4) Gd(1)-(8) 2.442(4) Gd(1)-(7) 2.471(5) Gd(1)-(11) 2.472(5) Gd(1)-(10) 2.513(4) Gd(1)-(2) 2.538(4) (1)-Gd(1)-(3) 69.45(14) (1)-Gd(1)-(2) 63.41(13) (3)-Gd(1)-(4) 62.51(13) (2)-Gd(1)-(4) (15) Bond angles around Nickel(II) ( ) Gd(1)-(4) 2.610(5) Bond lengths around Nickel(III) (Å) (1)-Ni(1)-(3) 81.48(17) (3)-Ni(1)-N(4) 87.41(18) (1)-Ni(1)-N(2) 87.26(18) N(4)-Ni(1)-N(2) (18) Ni(1)-(5) 2.017(4) Ni(1)-(1)-Gd(1) (17) Ni(1)-(1) 2.039(4) Ni(1)-(3)-Gd(1) (17) Ni(1)-(3) 2.047(4) Ni(1)-N(4) 2.069(5) S4
5 Ni(1)-(13) 2.094(4) Ni(1)-N(2) 2.127(5) S5
6 Table S4. Bond lengths around Bond angles around Erbium(III) Erbium(III) N 1 N 2 13 H N 5 9 (Å) ( ) Fe N 3 N 4 Ni Er N 6 12 Er(1)-(6) 2.270(5) Er(1)-(1) 2.278(6) Er(1)-(3) 2.299(5) Er(1)-(8) 2.385(6) Er(1)-(7) 2.401(7) Er(1)-(11) 2.425(6) Er(1)-(10) 2.465(6) Er(1)-(2) 2.520(6) (1)-Er(1)-(3) 70.6(2) (1)-Er(1)-(2) 64.27(19) (3)-Er(1)-(4) 62.80(19) (2)-Er(1)-(4) (19) Bond angles around Nickel(II) ( ) Er(1)-(4) 2.599(6) Bond lengths around Nickel(II) (Å) (1)-Ni(1)-(3) 80.7(2) (3)-Ni(1)-N(4) 87.7(2) (1)-Ni(1)-N(2) 87.2(2) N(4)-Ni(1)-N(2) 104.4(3) Ni(1)-(5) 2.004(5) Ni(1)-(1)-Er(1) 103.8(3) Ni(1)-(1) 2.033(6) Ni(1)-(3)-Er(1) 102.5(3) Ni(1)-(3) 2.051(6) Ni(1)-(13) 2.074(5) Ni(1)-N(4) 2.079(7) Ni(1)-N(2) 2.137(7) S6
7 Table S5. Bond lengths around Bond angles around Yttrium (III) Yttrium (III) Fe N 1 N 3 N 2 N 4 13 H 2 Ni Y N N 6 12 (Å) Y(1)-(6) 2.277(2) Y(1)-(1) 2.279(2) Y(1)-(3) 2.299(2) Y(1)-(8) 2.401(3) Y(1)-(7) 2.434(3) ( ) (1)-Y(1)-(2) 64.07(8) (3)-Y(1)-(4) 63.04(7) (2)-Y(1)-(4) (8) (1)-Y(1)-(3) 70.52(8) Y(1)-(10) 2.439(3) Y(1)-(11) 2.473(2) Y(1)-(2) 2.529(3) Y(1)-(4) 2.596(3) Bond angles around Nickel(II) ( ) Bond lengths around Nickel(II) (Å) Ni(1)-(5) 2.020(2) (1)-Ni(1)-(3) 80.77(9) (1)-Ni(1)-N(2) 87.51(9) N(4)-Ni(1)-N(2) (10) (3)-Ni(1)-N(4) 87.87(9) Ni(1)-(1) 2.036(2) Ni(1)-(1)-Y(1) (9) Ni(1)-(3) 2.043(2) Ni(1)-(3)-Y(1) (9) Ni(1)-N(4) 2.069(3) Ni(1)-(13) 2.086(2) Ni(1)-N(2) 2.123(3) S7
8 Y(1)-Ni(1) (11) S8
9 Figure S1. Molecular structure of 2. Hydrogen atoms and solvent molecules are omitted for clarity. S9
10 Figure S2. Molecular structure of 3. Hydrogen atoms and solvent molecules are omitted for clarity. Figure S3. Molecular structure of 4. Hydrogen atoms and solvent molecules are omitted for clarity. S10
11 Figure S4. Molecular structure of 5. Hydrogen atoms and solvent molecules are omitted for clarity. Figure S5. Molecular structure of 6. Hydrogen atoms and solvent molecules are omitted for clarity. S11
12 (a) (b) Figure S6. ESI-MS of 2.(a) Theoretical simulation (b) Experimental spectrum. (a) (b) Figure S7. ESI-MS of 3.(a) Theoretical simulation (b) Experimental spectrum. S12
13 (a) (b) Figure S8. ESI-MS of 4. (a) Theoretical simulation (b) Experimental spectrum. (a) (b) Figure S9. ESI-MS of 5. (a) Theoretical simulation (b) Experimental spectrum. S13
14 (a) (b) Figure S10. ESI-MS of 6. (a) Theoretical simulation (b) Experimental spectrum. Figure S11. Cyclic voltammogram of 1 in CH 2 Cl 2 using Glassy-Carbon working electrode and TBAP as supporting electrolyte (Scan rate 100mV/s). S14
15 Figure S12. Cyclic voltammogram of 3 in CH 2 Cl 2 using Glassy-Carbon working electrode and TBAP as supporting electrolyte (Scan rate 100mV/s). Figure S13. Cyclic voltammogram of 4 in CH 2 Cl 2 using Glassy-Carbon working electrode and TBAP as supporting electrolyte (Scan rate 100mV/s). S15
16 Uv-vis Spectra: The UV/Vis spectra of the ligand and the hetero metallic complexes were recorded at room temperature in CHCl 3 (c ~ 4.1X10-5 ). The observed λ max and corresponding ε max are summarized in Table S6. All the complexes shows similar type spectral features with a strong absorption around 284 nm along with two other transition around 354 nm and 444 nm, suggesting that these absorption bands arise due to spin allowed π-π* transitions in the ligand. Figure S14. UV/Vis absorption spectra of ligand (H 2 L) and complex (1-6). S16
17 Table S6. UV/Vis absorption data showing λ max value and corresponding ε max of ligand (H 2 L) and complex (1-6). Complex ligand Ni-Dy Ni-Tb Ni-Gd Ni-Ho Ni-Er Ni-Y λ max (nm)(10-306(2.23), 284(4.32), 284(3.12), 284(5.04), 284(4.21), 284(3.67), 286(4.38), 4 ε max ) 364(1.09), 354(1.80), 354(1.31), 355(2.07), (1.73), 354(1.5), 358(1.76), 469(0.25) 444(0.16) 443(0.15) (0.21) 451(0.17) 445(0.17) 450(0.11) Figure S15. Conformations of the 1,1 disubstitutedferrocene. a Synclinal (eclipsed) conformation corresponds to the situation where the two cyclopentadienyl groups are perfectly eclipsed while the 1,1 substituents on these rings are not. In anticlinal (staggered) conformation the two cyclopentadienyl rings as well as two substituents on the 1,1 positions are staggered. S17
18 Table S7. Torsion angle data for H 2 L and the complexes 1-6. Complex ligand Ni-Dy Ni-Tb Ni-Gd Ni-Ho Ni-Er Ni-Y θ 2.16(5) 2.14(8) 3.25(5) 2.71(5) 2.60(3) 2.50(6) S18
19 N N H 2 N Fe N N Ni Dy N Ni Dy Both Ni II and Dy III ion shares one four membered ring Dy N two four membered ring arround Dy III ion Dy two five membered ring arround Dy III ion Fe Ni N N Dy Both Ni II and Dy III ion shares two six membered ring N N Ni N Ni two six membered ring arround Ni II ion one ten membered ring arround Ni II ion Figure S16. Varying sizes of rings found in complex 1. S19
20 Figure S17.View of the H-bonds between two neighboring molecules of 4. S20
21 (a) Figure S18. (a) χt vs. T plots for Zn-Ln complexes (Ln = Tb, Dy and Ho); (b) M=f(H) plots at 2 K for the ferrocene based Zn-Ln complexes (Ln = Tb, Dy and Ho). 14 (b) S21
22 (a) (b) S22
23 (c) Figure S19. χ"= f(t) at dc field of 1000 e and ac field of 3 e at different frequencies for 1(a), 2(b) and 3(c) from top to down. S23
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