Tetrahedral Structure and Luminescence Properties of Bi-Metallic Pt 1 Ag 28 (SR) 18 (PPh 3 ) 4 Nanocluster
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1 Electronic Supplementary Material (ESI) for Chemical Science. This journal is The Royal Society of Chemistry 2017 Supporting Information: Tetrahedral Structure and Luminescence Properties of Bi-Metallic Pt 1 Ag 28 (SR) 18 (PPh 3 ) 4 Nanocluster Xi Kang, a Meng Zhou, b Shuxin Wang, a Shan Jin, a Guodong Sun, a Manzhou Zhu a,* & Rongchao Jin b,* a Department of Chemistry and Center for Atomic Engineering of Advanced Materials, Anhui University, Hefei, Anhui , China. b Department of Chemistry, Carnegie Mellon University, Pittsburgh, Pennsylvania 15213, United States. Structural analyses of Pt 1 Ag 28, Au 1 Ag 28 and Ag 29 Structurally, the previous studies suggested that the structure and composition of the metal core significantly affect the M S bond lengths. Thus the bond lengths and angles in Pt 1 Ag 28 were compared with the related ones in Ag 29 and Au 1 Ag 28 (Table S2). Compared the bond lengths in Pt 1 Ag 28 with Ag 29 and Au 1 Ag 28, the range is larger (Au 1 Ag 28 is similar with Ag 29 owing to the almost identified framework) although the average bond length is very similar. Regarding to the angles of P Ag S on the same motifs, the average angles of Ag 29 and Pt 1 Ag 28 is o and o, respectively. However the average angles in Pt 1 Ag 28 is , which varies substantially with Ag 29 (Au 1 Ag 28 ). Fig. S1. The total structure of Pt 1 Ag 28 (S Adm) 18 (PPh 3 ) 4. Color legend: green sphere, Pt; cerulean sphere, Ag on the shell; violet sphere, Ag in the kernel; red sphere, S; purple sphere, P. For clarity, C and H are shown in wireframe. s1
2 Fig. S2. a) UV Vis spectrum of Pt 1 Ag 28 ; b) MALDI MS spectrum of Pt 1 Ag 28 ; c) UV Vis spectrum of Pt 1 Ag 24 etching by Adm SH only ; d) MALDI MS spectrum of Pt 1 Ag 24 etching by Adm SH only. Fig. S3. X ray photoelectron spectroscopy (XPS) of a) Ag 3d, b) Pt 4f in Pt 1 Ag 28 (S Adm) 18 (PPh 3 ) 4 nanocluster. s2
3 Fig. S4. ESI MS mass spectrum of Pt 1 Ag 28 in positive mode. Insets: the experimental (black) and simulated (red) isotope patterns of Pt 1 Ag 28. Fig. S5. The M 13 kernel of a) Pt 1 Ag 28, b) Ag 29 and c) Au 1 Ag 28 nanoclusters. Color legend: green sphere, Pt; cerulean sphere, Ag. s3
4 Fig. S6. The motifs in Ag 29 and Au 1 Ag 28 nanoclusters. The overall motif could be separated into 4 Ag 1 S 3 P 1 and 4 Ag 3 S 3 motifs. Color legend: cerulean sphere, Ag; red sphere, S; purple sphere, P. Fig. S7. The motifs in Pt 1 Ag 28 nanocluster. The overall motif could be separated into 4 Ag 1 S 3 P 1 and 6 Ag 2 S 1 motifs or 4 Ag 4 S 6 P 1 motifs sharing 6 S atoms. Color legend: cerulean sphere, Ag; red sphere, S; purple sphere, P. Fig. S8. Total structure of a) Pt 1 Ag 28, b) Ag 29 and c) Au 1 Ag 28 nanoclusters. Color legend: green sphere, Pt; cerulean sphere, Ag; orange sohere, Au; red sphere, S; purple sphere, P. For clarity, C and H are not shown. s4
5 Fig. S9. Photoluminescence properties of Pt 1 Ag 28 (S Adm) 18 (PPh 3 ) 4. Excitation spectrum (left) and emission spectra (right) at different excitation wavelengths, as indicated by the arrows. Fig. S10. Femtosecond transient absorption data map at all time delays (0.1 ps to 3 ns) and probe wavelengths for a) Pt 1 Ag 24 and b) Pt 1 Ag 28 nanoclusters with excitation of 360 nm. c, d) Kinetic traces at selected wavelengths between 1 ps and 1 ns for c) Pt 1 Ag 24 and d) Pt 1 Ag 28. s5
6 Fig. S11. a) Femtosecond transient absorption data map of Pt 1 Ag 24 at early time delays ( 0.5 ps to 5 ps). b) Coherent oscillations observed in kinetic traces at selected wavelengths. Fig. S12. a) TGA curve and b) the derivative of Pt 1 Ag 24 ; c) TGA curve and d) the derivative of Pt 1 Ag 28. s6
7 Table S1. The atom ratio of Pt and Ag in Pt 1 Ag 28 (S Adm) 18 (PPh 3 ) 4 nanocluster calculated from inductively coupled plasma (ICP) and X ray photoelectric spectroscopy (XPS) measurements. Pt atom Ag atom ICP Experiment ratio of 3.9% 96.1% Pt 1 Ag 28 (S-Adm) 18 (PPh 3 ) 4 XPS Experiment ratio of 3.5% 96.5% Pt 1 Ag 28 (S-Adm) 18 (PPh 3 ) 4 Theoretical ratio of Pt 1 Ag 28 (S-Adm) 18 (PPh 3 ) 4 1/29(3.45%) 28/29(96.55%) Table S2. Structural analysis of Ag 29, Au 1 Ag 28 and Pt 1 Ag 28 nanoclusters. M(center) Ag lengths in the kernel (Å) Ag S lengths on the kernel shell (Å) Ag Ag lengths on the kernel shell (Å) P Ag S angles on the same motifs ( o ) Ag Averages Au 1 Ag Averages Pt 1 Ag Averages Table S3. Excited state lifetimes of silver and doped silver nanoclusters. Sample Excited State Lifetimes Ag 25 [1] Pt 1 Ag 24 Ag 29 [2] Pt 1 Ag μs 1.9 μs 350 ns 300 ns, 2.9 μs s7
8 Table S4: Crystal data and structure refinement for the Pt 1 Ag 28 (S Adm) 18 (PPh 3 ) 4 nanocluster. Compound reference Pt 1 Ag 28 (S Adm) 18 (PPh 3 ) 4 Empirical formula C252H330Ag28PtP4S18 Formula weight Temperature 143 K Wavelength Å Crystal system Monoclinic Space group C 2/c Unit cell dimensions A= (18) Å α=90 B= (8)Å β= (4) C= (16)Å γ=90 Volume 68775(4) Å 3 Z 8 Density (calculated) Mg m -3 Absorption coefficient mm -1 F(000) Crystal size mm 3 Theta range for data collection 3.01 to Index ranges -63<=h<=59, -34<=k<=36, -57<=l<=61 Reflections collected Independent reflections Absorption correction Multi scan Refinement method SHELXL-2014/7 (Sheldrick 2014/7) Data / restraints / parameters / 8 / 2728 Goodness-of-fit on F Final R indices [I>2sigma(I)] R1=0.0333, wr2= R indices (all data) R1=0.0432, wr2= References. [1] Bootharaju, M. S., Joshi, C. P., Parida, M. R., Mohammed, O. F. & Bakr, O. M. Templated atom precise galvanic synthesis and structure elucidation of a [Ag 24 Au(SR) 18 ] nanocluster. Angew. Chem. Int. Ed. 55, (2016). [2] Soldan, G., Aljuhani, M. A., Bootharaju, M. S., AbdulHalim, L. G., Parida, M. R., Emwas, A. H., Mohammed, O. F. & Bakr, O. M. Gold doping of silver nanoclusters: a 26 fold enhancement in the luminescence quantum yield. Angew. Chem. Int. Ed. 55, (2016). [3] AbdulHalim, L. G., Bootharaju, M. S., Tang, Q., Gobbo, S. D., AbdulHalim, R. G., Eddaoudi, M., Jiang, D. en. & Bakr, O. M. Ag 29 (BDT) 12 (TPP) 4 : a tetravalent nanocluster. J. Am. Chem. Soc. 137, (2015). s8
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