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1 advances.sciencemag.org/cgi/content/full/3/5/e /dc1 Supplementary Materials for Molecular surgery on a 23-gold-atom nanoparticle Qi Li, Tian-Yi Luo, Michael G. Taylor, Shuxin Wang, Xiaofan Zhu, Yongbo Song, Giannis Mpourmpakis, Nathaniel L. Rosi, Rongchao Jin This PDF file includes: Published 19 May 2017, Sci. Adv. 3, e (2017) DOI: /sciadv X-ray Experimentals fig. S1. UV-Vis absorption spectra of [Au23(SR)16] and [Au23 xagx(sr)16]. fig. S2. MALDI mass spectra of [Au23(SR)16] (black), [Au23 xagx(sr)16] (green), and [Au21(SR)12(P C P)2] + (gray) sample. fig. S3. ESI mass spectrum of [Au21(SR)12(P C P)2] +. fig. S4. 31 P-NMR spectrum of [Au21(SR)12(P C P)2] +. fig. S5. UV-Vis absorption spectra of samples with increasing mass ratio of Ag I (SR) that reacted with [Au23(SR)16]. fig. S6. X-ray crystal structure of [Au25 xagx(sr)18] (x ~ 4). fig. S7. Ag I (SR) complex induced transformation from [Au23(SR)16] to heavily Ag-doped [Au25 xagx(sr)18]. fig. S8. DFT-relaxed [Au23 xagx(sr)18] (x = 1 to 3) and [Au25 yagy(sr)18] (y = 2, 3) nanoclusters and associated relative electronic energies. table S1. Atomic percentages of Au and Ag in the [Au21(SR)12(P C P)2] + [AgCl2] obtained by EDS-SEM. table S2. DFT free energies of reactions of intermediates and possible reaction pathways. table S3. Crystal data and structure refinement for Au22.13Ag0.87(SR)16 TOA +. table S4. Crystal data and structure refinement for Au20.51Ag4.49(SR)18 TOA +. table S5. Crystal data and structure refinement for [Au21(SR)12(P C P)2] + [AgCl2].
2 X-ray Experimentals Crystallographic Determination of [Au21(SR)12(P C P)2] + [AgCl2] - Single crystal X-ray diffraction data of [Au21(SR)12(P C P)2] + [AgCl2] - was collected on a Bruker X8 Prospector Ultra diffractometer equipped with an Apex II CCD detector and an IµS microfocus CuKα X-ray source (λ = Å). A piece of dark brown block crystal with dimensions 0.18 x 0.12 x 0.04 mm was mounted onto a MiTeGen micro-mount. Data collection was performed at K. A triclinic unit cell with a = (6) Å, b = (6) Å, c = (13) Å, α = (2), β = (2)º, γ = (10) o was determined using the least-square refinement. The frames were integrated with the Bruker SAINT software package reflections in the range < 2θ < was collected, of which were independent. (average redundancy 3.57, completeness = 96.4 %, Rint = 6.40 %, Rsigma = 5.95 %) Data were corrected for absorption effects using SADABS Multi-Scan method (Tmax = 0.753, Tmin = 0.300). The structure was solved by intrinsic phasing using Bruker program SHELXT. All the Au, Ag, S, Cl and P atoms were found directly. Remaining non-hydrogen atoms were generated via subsequent difference Fourier syntheses. All of the non-hydrogen atoms were refined anisotropically. SADI restraints were used to optimize the bond lengths and angles of some cyclohexyl groups. SIMU and RIGU restraints were applied to refine ellipsoids of some carbon atoms. Idealized hydrogen atom positions were calculated. The electron densities corresponding to the disordered molecules in the void were flattened by SQUEEZE procedure in PLATON. Crystallographic Determination of Au22.13Ag0.87(SR)16 TOA + Single crystal X-ray diffraction data of Au22.13Ag0.87(SR)16 TOA + was collected on a Bruker X8 Prospector Ultra diffractometer equipped with an Apex II CCD detector and an IµS micro-focus CuKα X-ray source (λ = Å). A piece of dark brown block crystal with dimensions 0.06 x 0.03 x 0.01 mm was mounted onto a MiTeGen micromount. Data collection was performed at K. A base-centered orthorhombic unit cell with a = (9) Å, b = (18) Å, c = (7) Å, α = β =γ = 90 o was determined using the least-square refinement. The frames were integrated with the Bruker SAINT software package reflections in the range 2.78 < 2θ < were collected, of which were independent (average redundancy 8.90, completeness = 99.8%, Rint = 15.30%, Rsigma = 7.57% ) Data were corrected for absorption effects using SADABS Multi-Scan method (Tmin = 0.373, Tmax = 0.750). Centrosymmetric space group Ccca was determined based on systematic absences. The structure was solved by intrinsic phasing using Bruker program SHELXT. The asymmetric unit contains two crystallographically independent clusters each siting on an inversion center. All the metal and S atoms were found directly. Remaining non-hydrogen atoms were generated via subsequent difference Fourier syntheses. All of the non-hydrogen atoms were refined anisotropically. SADI restraints were used to optimize the bond lengths and angles of some cyclohexyl groups. SIMU and RIGU restraints were applied to refine ellipsoids of some carbon atoms. Idealized hydrogen atom positions were calculated. Tetraoctylammonium cation was found to be coexisting with the cluster. However, some tail carbon atoms could not be located due to severe disorder.
3 There are 24 metal atom positions in the asymmetric unit. Therefore, 24 free variables were introduced to represent the occupancies of Ag atoms at these positions. EXYZ and EADP was used to restrain Ag and Au atoms at the same position to have the same coordinates and thermal displacement. After refinement, 19 out of these 24 free variables were slightly negative, indicating 0% occupancy for Ag and 100% occupancy for Au at these sites. Therefore, these 19 free variables were removed and these 19 sites were treated as 100% Au atoms, while the occupancy values for other 5 metal positions were further refined using 5 free variables. Crystallographic Determination of Au20.51Ag4.49(SR)18 TOA + Single crystal X-ray diffraction data of Au20.51Ag4.49(SR)18 TOA + was collected on a Bruker X8 Prospector Ultra diffractometer equipped with an Apex II CCD detector and an IµS micro-focus CuKα X-ray source (λ = Å). A piece of dark brown block crystal with dimensions 0.08 x 0.04 x 0.02 mm was mounted onto a MiTeGen micromount. Data collection was performed at K. A base-centered monoclinic unit cell with a = (19) Å, b = (18) Å, c = (2) Å, α = γ = 90 o, β = (6)º was determined using the least-square refinement. The frames were integrated with the Bruker SAINT software package reflections in the range < 2θ < were collected, of which 8484 were independent (average redundancy 3.98, completeness = 98.5%, Rint = 7.25%, Rsigma = 6.12% ) Data were corrected for absorption effects using SADABS Multi-Scan method (Tmin = 0.354, Tmax = 0.750). Centrosymmetric space group C2/c was determined based on systematic absences. The structure was solved by intrinsic phasing using Bruker program SHELXT. All the metal and S atoms were found directly. Remaining non-hydrogen atoms were generated via subsequent difference Fourier syntheses. All of the nonhydrogen atoms were refined anisotropically. SADI restraints were used to optimize the bond lengths and angles of some cyclohexyl groups. SIMU and RIGU restraints were applied to refine ellipsoids of some carbon atoms. Idealized hydrogen atom positions were calculated. Tetraoctylammonium cation was not found due to its disorder in voids. There are 13 metal atom positions, one of which sits on an inversion center, in the asymmetric unit. Therefore, 13 free variables were introduced to represent the occupancies of Au atoms at these positions. EXYZ and EADP was used to restrain Ag and Au atoms at the same position to have the same coordinates and thermal displacement. After refinement, free variables at 7 different positions representing Au occupancies were calculated slightly greater than 100%, indicating 100% occupancy for Au and 0% occupancy for Ag at these sites. Therefore, these 7 free variables were removed and these 7 sites were treated as 100% Au atoms, while the occupancy values for other 6 metal positions were further refined using 6 free variables.
4 fig. S1. UV-Vis absorption spectra of [Au23(SR)16] and [Au23 xagx(sr)16]. fig. S2. MALDI mass spectra of [Au23(SR)16] (black), [Au23 xagx(sr)16] (green), and [Au21(SR)12(P C P)2] + (gray) sample. (a) An intense peak at ~6375 Da is assigned to the intact [Au23(SR)16], (theoretical value: Da). Intense peaks of [Au22Ag1(SR)16] and [Au21Ag2(SR)16] can be observed at ~ 6285 Da and ~ 6196 Da from the [Au23-xAgx(SR)16] (x: 0~2) sample. (b) An intense peak at ~ 6288 Da is assigned to the intact [Au21(SR)12(P-C-P)2] +, (theoretical value: Da). Note: fragmentation was found in all the three samples, of which the intensity show a laser power dependence. In the spectra of [Au21(SR)12(P-C-P)2] +, the space of fragments and intact nanocluster is (AuSR)n (n: 1-4). [Au23(SR)16] and [Au23-xAgx(SR)16] - samples were conducted by negative mode; [Au21(SR)12(P-C-P)2] + sample was done in positive mode.
5 fig. S3. ESI mass spectrum of [Au21(SR)12(P C P)2] +. (a) The signal at Da suggests the intact [Au21(SR)12(P-C-P)2] + cluster. No silver-doped [Au21(SR)12(P-C-P)2] + could be identified, suggesting all the dopants (silver) were pulled out. (b) Zoom-in ESI mass spectrum which shows the isotrope pattern. The experimental data (black) is consistent with the simulated pattern (grey). The 1 Da spacing of the isotropic peaks suggests +1 charge of the Au21 cluster. The measurement was done in positive mode. fig. S4. 31 P-NMR spectrum of [Au21(SR)12(P C P)2] +.
6 fig. S5. UV-Vis absorption spectra of samples with increasing mass ratio of Ag I (SR) that reacted with [Au23(SR)16]. (a) Scheme of the reaction between [Au23(SR)16] and Ag I (SR) complex. Magenta: Au, yellow: S. All the C and H have been deleted for clarity. (b) UV/Vis absorption spectra of samples with increasing mass ratio of Ag I (SR) reacted with [Au23(SR)16]. The relative mass of [Au23(SR)16] is set to be 1. fig. S6. X-ray crystal structure of [Au25 xagx(sr)18] (x ~ 4). 13-atom icosahedral alloy core is shown on the left, in which the 12 atoms on the icosahedral inner shell are occupied by Ag with variable occupancies. The (AuAg)25S18 framework is shown on the right and no Ag can be found on the motif. The percentages of Ag on the icosahedral inner shell are Ag2 : 48.4%, Ag3 : 37.1%; Ag4 : 33.1%; Ag5 : 34.8%; Ag6 : 21.2%; Ag7: 49.9%. The X-ray crystallography averaged composition is determined to be Au20.51Ag4.49SR18 -.Magenta: Au, gray: Ag, yellow: S. This result suggest that the Ag prefer to locate on the icosahedral inner shell in AuAg25 cluster.
7 fig. S7. Ag I (SR) complex induced transformation from [Au23(SR)16] to heavily Ag-doped [Au25 xagx(sr)18]. Two intermediate products: [Au23-xAgx(SR)16] (x: 0~2) and [Au25- xagx(sr)18] (x~4) were defined by X-ray single crystal analysis and a doping-growth-doping mechanism was observed. Magenta: Au, gray: Ag, yellow: S, C and all H atoms have been deleted for clarity.
8 fig. S8. DFT-relaxed [Au23 xagx(sr)18] (x = 1 to 3) and [Au25 yagy(sr)18] (y = 2, 3) nanoclusters and associated relative electronic energies. Carbon and hydrogen atoms have been removed for clarity. Color code: Pink=Au, Yellow=S, Silver=Ag. In (a-f), x=1 and (a) and (b) represent the positions observed in X-ray Diffraction experiments (see Fig. 2). In (g-i), x=2, in (j), x=3, in (k), y=2, and in (l), y=3.
9 table S1. Atomic percentages of Au and Ag in the [Au21(SR)12(P C P)2] + [AgCl2] obtained by EDS-SEM. Several [Au21(SR)12(P-C-P)2] + [AgCl2] - crystals were tested and the average Au/Ag value was calculated. The inset picture is a SEM image of a typical crystal. Atomic Percent Obtained by Energy Dispersive X-ray Gold and Silver Atoms Normalized to 21 Gold Atoms Gold Silver Gold Silver Average
10 table S2. DFT free energies of reactions of intermediates and possible reaction pathways. All free energies are calculated at K and are reported for the minimum-energy isomers unless otherwise stated. Primary Reacting Species [Au23SR16] - Reaction Type Grxn (kcal/mol) [Au23SR16] - + ¼ Ag4SR4 [Au22AgSR16] - + ¼ Ag Doping Au4SR4 [Au23SR16] - + ½ Ag4SR4 [Au23Ag2SR18] - Ag Growth [Au23SR16] - + 2(AuCl)2 PPh2CPPh2 Au4SR4 + [Au21(SR)12(Ph2PCH2PPh2)2(AuCl2)2] - Motif-Exchange 4.44 [Au23SR16] - + ½ Au4SR4 [Au25SR18] - Au Growth 5.47 [Au22AgSR16] - [Au22AgSR16] - + ¼ Ag4SR4 [Au21Ag2SR16] - + Ag Doping [Au22AgSR16] - + ½ Ag4SR4 [Au22Ag3SR18] - Ag Growth [Au21Ag2SR16] - [Au21Ag2SR16] - + ½ Ag4SR4 [Au21Ag4SR18] - Ag Growth [Au21Ag2SR16] - + ¼ Ag4SR4 [Au20Ag3SR16] - + Ag Doping (Figure S7(g) [Au21Ag2SR16] - + 2(AuCl)2 PPh2CPPh2 Motif-Exchange 6.50 isomer) Au4SR4 + [Au21(SR)12(Ph2PCH2PPh2)2(AgCl2)2] - (Figure S7(h) [Au21Ag2SR16] - + 2(AuCl)2 PPh2CPPh2 Motif-Exchange 3.30 isomer) Au4SR4 + [Au21(SR)12(Ph2PCH2PPh2)2(AgCl2)2] - (Figure S7(i) [Au21Ag2SR16] - + 2(AuCl)2 PPh2CPPh2 Motif-Exchange 1.03 isomer) Au4SR4 + [Au21(SR)12(Ph2PCH2PPh2)2(AgCl2)2] - [Au20Ag3SR16] - [Au20Ag3SR16] - + ½ Ag4SR4 [Au20Ag5SR18] - Ag Growth [Au20Ag3SR16] - + ¼ Ag4SR4 [Au19Ag4SR16] - + Ag Doping [Au25SR18] - [Au25SR18] - + ¼ Ag4SR4 [Au24AgSR18] - + ¼ Ag Doping Au4SR4 [Au24AgSR18] - [Au24AgSR18] - + ¼ Ag4SR4 [Au23Ag2SR18] - + [Au23Ag2SR18] - [Au23Ag2SR18] - + ¼ Ag4SR4 [Au22Ag3SR18] - + [Au22Ag3SR18] - [Au22Ag3SR18] - + ¼ Ag4SR4 [Au21Ag4SR18] - + [Au21Ag4SR18] - [Au21Ag4SR18] - + ¼ Ag4SR4 [Au20Ag5SR18] - + Ag Doping Ag Doping Ag Doping Ag Doping -4.51
11 table S3. Crystal data and structure refinement for Au22.13Ag0.87(SR)16 TOA +. Empirical formula C117H210Ag0.87Au22.13NS16 Formula weight Temperature/K Crystal system orthorhombic Space group Ccce a/å (9) b/å (18) c/å (7) α/ 90 β/ 90 γ/ 90 Volume/Å (3) Z 16 ρcalcg/cm μ/mm F(000) Crystal size/mm Radiation CuKα λ = Θ range for data collection/ 2.78 to Index ranges -33 h 33, -64 k 64, -20 l 32 Reflections collected Independent reflections [Rint = , Rsigma = ] Data/restraints/parameters 18500/1257/1423 Goodness-of-fit on F Final R indexes [I>=2σ (I)] R1 = , wr2 = Final R indexes [all data] R1 = , wr2 = Largest diff. peak/hole / e Å /-1.03
12 table S4. Crystal data and structure refinement for Au20.51Ag4.49(SR)18 TOA +. Identification code 4_23_16LTYAUAG25LQ_0m_a Empirical formula C108H198Ag4.49Au20.51S18 Formula weight Temperature/K Crystal system monoclinic Space group C2/c a/å (19) b/å (18) c/å (2) α/ 90 β/ (6) γ/ 90 Volume/Å (2) Z 4 ρcalcg/cm μ/mm F(000) Crystal size/mm Radiation CuKα (λ = ) 2Θ range for data collection/ to Index ranges 25 h 25, 23 k 23, 24 l 27 Reflections collected Independent reflections 8484 [Rint = , Rsigma = ] Data/restraints/parameters 8484/227/688 Goodnessoffit on F Final R indexes [I>=2σ (I)] R1 = , wr2 = Final R indexes [all data] R1 = , wr2 = Largest diff. peak/hole / e Å /1.04
13 table S5. Crystal data and structure refinement for [Au21(SR)12(P C P)2] + [AgCl2]. Identification code ltylq _0m_a Empirical formula C61H88Ag0.5Au10.5ClP2S6 Formula weight Temperature/K Crystal system triclinic Space group P-1 a/å (6) b/å (6) c/å (13) α/ (2) β/ (2) γ/ (10) Volume/Å (5) Z 4 ρ calcg/cm μ/mm F(000) Crystal size/mm Radiation CuKα (λ = ) 2Θ range for data collection/ to Index ranges -19 h 19, -20 k 20, -36 l 38 Reflections collected Independent reflections [Rint = , Rsigma = ] Data/restraints/parameters 27821/536/1462 Goodness-of-fit on F Final R indexes [I>=2σ (I)] R1 = , wr2 = Final R indexes [all data] R1 = , wr2 = Largest diff. peak/hole / e Å /-5.86
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