A Correlated Series of Au/Ag Nanoclusters Revealing the Evolutionary Patterns of Asymmetric Ag Doping.
Li, Yingwei; Luo, Tian-Yi; Zhou, Meng; Song, Yongbo; Rosi, Nathaniel L.; Jin, Rongchao; Journal of the American Chemical Society 140 (2018) 14235–14243; doi:10.1021/jacs.8b08335

data_4133064
_publ_section_title
;
 A Correlated Series of Au/Ag Nanoclusters Revealing the Evolutionary
 Patterns of Asymmetric Ag Doping.
;
_journal_issue                   43
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14235
_journal_page_last               14243
_journal_paper_doi               10.1021/jacs.8b08335
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C150 H225 Ag7.44 Au15.56 S15'
_chemical_formula_sum            'C150 H225 Ag7.85 Au15.15 S15'
_chemical_formula_weight         6340.38
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            12
_cell_length_a                   28.5598(9)
_cell_length_b                   28.5598(9)
_cell_length_c                   73.154(4)
_cell_measurement_reflns_used    7042
_cell_measurement_temperature    229.9
_cell_measurement_theta_max      36.42
_cell_measurement_theta_min      3.01
_cell_volume                     51675(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      229.91
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II CCD'
_diffrn_measured_fraction_theta_full 0.265
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1652
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.265
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            34343
_diffrn_reflns_point_group_measured_fraction_full 0.265
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         36.491
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'IMuS micro-focus source'
_diffrn_source_target            Cu
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    32.551
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.2718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1632 before and 0.0845 after correction. The Ratio of minimum to maximum transmission is 0.3638. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.445
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             35171
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.295
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         2763
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+14157.5029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1557
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2109
_reflns_number_total             2763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08335_si_005.cif
_cod_data_source_block           ltylyw20171007_2to1_0m_a
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4133064
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{Au2, Ag2}
{Au3, Ag3}
{Au5, Ag5}
{Au9, Ag9}
3. Restrained distances
 C22-C23
 1.54 with sigma of 0.02
 C46-C45
 1.54 with sigma of 0.02
 C29-C28 \\sim C24-C25
 with sigma of 0.02
 C25-C26 \\sim C23-C22 \\sim C28-C27
 with sigma of 0.02
 C28-C30 \\sim C25-C30
 with sigma of 0.02
 C22-C21 \\sim C27-C21 \\sim C26-C21
 with sigma of 0.02
 C44-C43 \\sim C50-C48 \\sim C46-C41
 with sigma of 0.02
 C48-C45 \\sim C49-C43 \\sim C47-C41
 with sigma of 0.02
 C17-C14 \\sim C18-C13
 with sigma of 0.02
 C20-C18 \\sim C20-C13
 with sigma of 0.02
 C13-C18 \\sim C12-C19
 with sigma of 0.02
 C35-C37 \\sim C40-C38
 with sigma of 0.02
 C19-C18 \\sim C13-C12 \\sim C16-C15 \\sim C16-C11 \\sim C19-C11 \\sim C12-C11
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim
C19 \\sim C20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim
C29 \\sim C30: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Au2) = Uanis(Ag2)
Uanis(Au3) = Uanis(Ag3)
Uanis(Au5) = Uanis(Ag5)
Uanis(Au9) = Uanis(Ag9)
5. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C14, C15, C16, C17, C18, C19, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24, C25, C26, C27, C28, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32, C33, C34, C35, C36, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, C42, C43, C44, C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(Ag2)=1-FVAR(1)
 Sof(Au2)=FVAR(1)
 Sof(Ag3)=1-FVAR(2)
 Sof(Au3)=FVAR(2)
 Sof(Ag5)=1-FVAR(3)
 Sof(Au5)=FVAR(3)
 Sof(Ag9)=1-FVAR(4)
 Sof(Au9)=FVAR(4)
7.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C13(H13), C15(H15), C18(H18), C23(H23), C25(H25),
 C28(H28), C35(H35), C37(H37), C39(H39), C43(H43), C45(H45), C50(H50)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,
 H10B), C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B),
 C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C26(H26A,H26B),
  C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B), C40(H40A,H40B),
 C42(H42A,H42B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B),
  C49(H49A,H49B)
;
_shelx_res_checksum              50741
_shelx_hkl_checksum              96548
_olex2_submission_special_instructions 'No special instructions were received'