Ligand-Stabilized Au13Cux (x= 2, 4, 8) Bimetallic Nanoclusters: Ligand Engineering to Control the Exposure of Metal Sites
Huayan Yang; Yu Wang; Jing Lei; Lei Shi; Xiaohu Wu; Ville Mäkinen; Shuichao Lin; Zichao Tang; Jian He; Hannu Häkkinen; Lansun Zheng; Nanfeng Zheng; Journal of the American Chemical Society 135 (2013) 9568–9571; doi:10.1021/ja402249s

data_4120006
_publ_contact_author_address
;
State Key Laboratory of Physical Chemistry of Solid Surfaces 
and Department of Chemistry
Xiamen University
422 Siming South Road
Xiamen, Fujian 361005
P. R. China
http://210.34.14.15/kydw_ktz/nfzheng/index.html
;
_publ_contact_author_email       nfzheng@xmu.edu.cn
_publ_contact_author_fax         +86-592-2183047
_publ_contact_author_name        'Nanfeng Zheng'
_publ_contact_author_phone       +86-592-2186821
_publ_section_title
;
 Ligand-Stabilized Au13Cux (x= 2, 4, 8) Bimetallic Nanoclusters: Ligand
 Engineering to Control the Exposure of Metal Sites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9568
_journal_page_last               9571
_journal_paper_doi               10.1021/ja402249s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         '8(C148 H160 Au13 Cu4 N4 P4 S8), 8(Cl O4)'
_chemical_formula_sum            'C150 H200 Au13 Cl Cu N O P8 S4'
_chemical_formula_weight         5068.66
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.75(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   42.633(8)
_cell_length_b                   22.6801(18)
_cell_length_c                   41.556(6)
_cell_measurement_reflns_used    13239
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      67.3260
_cell_measurement_theta_min      3.6170
_cell_volume                     35560(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.3415
_diffrn_measured_fraction_theta_full 0.9950
_diffrn_measured_fraction_theta_max 0.9950
_diffrn_measurement_details
;
  1 omega  -68.00   28.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299   57.0000   30.0000 96

  2 omega -110.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299  -57.0000 -120.0000 90

  3 omega  -48.00   15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9299   38.0000 -180.0000 63

  4 omega   55.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9299 -125.0000 -180.0000 41

  5 omega  -11.00   16.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   30.0000 -150.0000 27

  6 omega  -43.00   11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000   45.0000  120.0000 54

  7 omega  141.00  167.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  125.0000   30.0000 26

  8 omega   31.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000   60.0000 47

  9 omega   93.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   30.0000 -180.0000 85

 10 omega  132.00  174.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  125.0000   90.0000 42

 11 omega   30.00   76.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000   30.0000 46

 12 omega   43.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000  150.0000 32

 13 omega   69.00  121.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940 -125.0000    0.0000 52

 14 omega   33.00   62.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000 -120.0000 29

 15 omega   47.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000  150.0000 62

 16 omega   24.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000   60.0000 85

 17 omega   87.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940   30.0000   90.0000 90

 18 omega   47.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -94.0000 -120.0000 47

 19 omega   31.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000  -90.0000 55

 20 omega   37.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -30.0000 -180.0000 52

 21 omega  122.00  163.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  125.0000 -150.0000 41

 22 omega   36.00   74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.1940  -61.0000  150.0000 38
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0375440000
_diffrn_orient_matrix_UB_12      -0.0254815000
_diffrn_orient_matrix_UB_13      0.0146992000
_diffrn_orient_matrix_UB_21      0.0020518000
_diffrn_orient_matrix_UB_22      -0.0079435000
_diffrn_orient_matrix_UB_23      0.0379564000
_diffrn_orient_matrix_UB_31      -0.0151101000
_diffrn_orient_matrix_UB_32      -0.0626353000
_diffrn_orient_matrix_UB_33      -0.0105758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            115608
_diffrn_reflns_theta_full        67.08
_diffrn_reflns_theta_max         67.08
_diffrn_reflns_theta_min         3.68
_diffrn_source                   'SuperNova (Cu) x-ray Source'
_exptl_absorpt_coefficient_mu    2.661
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.23066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    0.237
_exptl_crystal_description       block
_exptl_crystal_F_000             2372
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
SQUEEZE removed 5 disordered dichloromethane and three water molecules per 
formula unit. 
;
_refine_diff_density_max         3.037
_refine_diff_density_min         -3.044
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1657
_refine_ls_number_reflns         31589
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0882P)^2^+1246.2900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1894
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                23133
_reflns_number_total             31589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja402249s_si_002.cif
_cod_data_source_block           XMC-5
_cod_original_cell_volume        35560(8)
_cod_database_code               4120006
_reflns_odcompleteness_completeness 99.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97