Probing the surface-active sites of metal nanoclusters with atomic precision: a case study of Au<sub>5</sub>Ag<sub>11</sub>.
Cao, Yaoyao; Xu, Ying; Shen, Honglei; Pan, Peiyao; Zou, Xuejuan; Kang, Xi; Zhu, Manzhou; Nanoscale 15 (2023) 13784–13789; doi:10.1039/d3nr03288d

data_1569670
_publ_section_title
;
 Probing the surface-active sites of metal nanoclusters with atomic
 precision: a case study of Au<sub>5</sub>Ag<sub>11</sub>.
;
_journal_issue                   33
_journal_name_full               Nanoscale
_journal_page_first              13784
_journal_page_last               13789
_journal_paper_doi               10.1039/d3nr03288d
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety         'C120 H80 Ag11 Au5 Cl16 O2 P4 S8'
_chemical_formula_sum            'C120 H80 Ag11.27 Au4.73 Cl16 O2 P4 S8'
_chemical_formula_weight         4648.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-05-10 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   23.4047(7)
_cell_length_b                   56.3203(16)
_cell_length_c                   46.1622(18)
_cell_measurement_reflns_used    59041
_cell_measurement_temperature    120
_cell_measurement_theta_max      69.71
_cell_measurement_theta_min      4.81
_cell_volume                     60849(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)'
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details      '2201 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1084
_diffrn_reflns_av_unetI/netI     0.1119
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -64
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            74458
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        62.500
_diffrn_reflns_theta_max         62.500
_diffrn_reflns_theta_min         3.526
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    24.022
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             34871
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.269
_refine_diff_density_min         -1.944
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         23986
_refine_ls_number_restraints     1440
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1605
_refine_ls_R_factor_gt           0.1193
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3143
_refine_ls_wR_factor_ref         0.3458
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12811
_reflns_number_total             23986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03288d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1569669--1569671.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1569670
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.645
_shelx_estimated_absorpt_t_min   0.123
_olex2_refinement_description
;
1. Shared sites
{Ag1, Au2}
2. Uiso/Uaniso restraints and constraints
C01I \\sim C01O \\sim C02J \\sim C01X \\sim C03U \\sim C02P \\sim C01K \\sim
C02N \\sim C029 \\sim C033 \\sim C035 \\sim C022 \\sim C01L \\sim C03G \\sim
C042 \\sim C030 \\sim C02H \\sim C01J \\sim C01N \\sim C01M \\sim C03M \\sim
C04T \\sim C045 \\sim C021 \\sim C01R \\sim C036 \\sim C04C \\sim C02M \\sim
C03V \\sim C02D \\sim C01W \\sim C04A \\sim C031 \\sim C03O \\sim C02Y \\sim
C01V \\sim C01Z \\sim C04D \\sim C02Z \\sim C02L \\sim C037 \\sim C01Q \\sim
C028 \\sim C049 \\sim C026 \\sim C03H \\sim C025 \\sim C024 \\sim C02B \\sim
C040 \\sim C03N \\sim C04B \\sim C02W \\sim C03S \\sim C02K \\sim C04R \\sim
C04O \\sim C04P \\sim C02I \\sim C020 \\sim C02O \\sim C01U \\sim C03Q \\sim
C02S \\sim C027 \\sim C02T \\sim C02Q \\sim C02E \\sim C01T \\sim C04U \\sim
C71 \\sim C04M \\sim C02U \\sim C02C \\sim C03D \\sim C02V \\sim C023 \\sim
C02X \\sim C034 \\sim C04K \\sim C03J \\sim C03W \\sim C04E \\sim C03C \\sim
C03A \\sim C03R \\sim C02G \\sim C04H \\sim C046 \\sim C041 \\sim C03B \\sim
C03Z \\sim C04G \\sim C04Q \\sim C03K \\sim C02R \\sim C03P \\sim C01S \\sim
C032 \\sim C62 \\sim C04L \\sim C04I \\sim C03T \\sim C47 \\sim C29 \\sim C044
\\sim C03F \\sim C039 \\sim C047 \\sim C49 \\sim C15 \\sim C25 \\sim C80 \\sim
C26 \\sim C048 \\sim C03Y \\sim C03E \\sim C03L \\sim C45 \\sim C04J: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C01I) \\sim Ueq, Uanis(C01O) \\sim Ueq, Uanis(C02J) \\sim Ueq,
Uanis(C01X) \\sim Ueq, Uanis(C03U) \\sim Ueq, Uanis(C02P) \\sim Ueq,
Uanis(C01K) \\sim Ueq, Uanis(C02N) \\sim Ueq, Uanis(C029) \\sim Ueq,
Uanis(C033) \\sim Ueq, Uanis(C035) \\sim Ueq, Uanis(C022) \\sim Ueq,
Uanis(C01L) \\sim Ueq, Uanis(C03G) \\sim Ueq, Uanis(C042) \\sim Ueq,
Uanis(C030) \\sim Ueq, Uanis(C02H) \\sim Ueq, Uanis(C01J) \\sim Ueq,
Uanis(C01N) \\sim Ueq, Uanis(C01M) \\sim Ueq, Uanis(C03M) \\sim Ueq,
Uanis(C04T) \\sim Ueq, Uanis(C045) \\sim Ueq, Uanis(C021) \\sim Ueq,
Uanis(C01R) \\sim Ueq, Uanis(C036) \\sim Ueq, Uanis(C04C) \\sim Ueq,
Uanis(C02M) \\sim Ueq, Uanis(C03V) \\sim Ueq, Uanis(C02D) \\sim Ueq,
Uanis(C01W) \\sim Ueq, Uanis(C04A) \\sim Ueq, Uanis(C031) \\sim Ueq,
Uanis(C03O) \\sim Ueq, Uanis(C02Y) \\sim Ueq, Uanis(C01V) \\sim Ueq,
Uanis(C01Z) \\sim Ueq, Uanis(C04D) \\sim Ueq, Uanis(C02Z) \\sim Ueq,
Uanis(C02L) \\sim Ueq, Uanis(C037) \\sim Ueq, Uanis(C01Q) \\sim Ueq,
Uanis(C028) \\sim Ueq, Uanis(C049) \\sim Ueq, Uanis(C026) \\sim Ueq,
Uanis(C03H) \\sim Ueq, Uanis(C025) \\sim Ueq, Uanis(C024) \\sim Ueq,
Uanis(C02B) \\sim Ueq, Uanis(C040) \\sim Ueq, Uanis(C03N) \\sim Ueq,
Uanis(C04B) \\sim Ueq, Uanis(C02W) \\sim Ueq, Uanis(C03S) \\sim Ueq,
Uanis(C02K) \\sim Ueq, Uanis(C04R) \\sim Ueq, Uanis(C04O) \\sim Ueq,
Uanis(C04P) \\sim Ueq, Uanis(C02I) \\sim Ueq, Uanis(C020) \\sim Ueq,
Uanis(C02O) \\sim Ueq, Uanis(C01U) \\sim Ueq, Uanis(C03Q) \\sim Ueq,
Uanis(C02S) \\sim Ueq, Uanis(C027) \\sim Ueq, Uanis(C02T) \\sim Ueq,
Uanis(C02Q) \\sim Ueq, Uanis(C02E) \\sim Ueq, Uanis(C01T) \\sim Ueq,
Uanis(C04U) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C04M) \\sim Ueq, Uanis(C02U)
\\sim Ueq, Uanis(C02C) \\sim Ueq, Uanis(C03D) \\sim Ueq, Uanis(C02V) \\sim Ueq,
Uanis(C023) \\sim Ueq, Uanis(C02X) \\sim Ueq, Uanis(C034) \\sim Ueq,
Uanis(C04K) \\sim Ueq, Uanis(C03J) \\sim Ueq, Uanis(C03W) \\sim Ueq,
Uanis(C04E) \\sim Ueq, Uanis(C03C) \\sim Ueq, Uanis(C03A) \\sim Ueq,
Uanis(C03R) \\sim Ueq, Uanis(C02G) \\sim Ueq, Uanis(C04H) \\sim Ueq,
Uanis(C046) \\sim Ueq, Uanis(C041) \\sim Ueq, Uanis(C03B) \\sim Ueq,
Uanis(C03Z) \\sim Ueq, Uanis(C04G) \\sim Ueq, Uanis(C04Q) \\sim Ueq,
Uanis(C03K) \\sim Ueq, Uanis(C02R) \\sim Ueq, Uanis(C03P) \\sim Ueq,
Uanis(C01S) \\sim Ueq, Uanis(C032) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C04L)
\\sim Ueq, Uanis(C04I) \\sim Ueq, Uanis(C03T) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C044) \\sim Ueq, Uanis(C03F) \\sim Ueq, Uanis(C039)
\\sim Ueq, Uanis(C047) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C048)
\\sim Ueq, Uanis(C03Y) \\sim Ueq, Uanis(C03E) \\sim Ueq, Uanis(C03L) \\sim Ueq,
Uanis(C45) \\sim Ueq, Uanis(C04J) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Ag1) = Uanis(Au2)
3. Others
 Sof(Au2)=1-FVAR(1)
 Sof(Ag1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C01O(H01O), C02J(H02J), C01X(H01X), C03U(H03U), C02P(H02P), C029(H029),
 C033(H033), C035(H035), C022(H022), C03G(H03G), C042(H042), C030(H030),
 C02H(H02H), C03M(H03M), C04T(H04T), C045(H045), C036(H036), C04C(H04C),
 C02M(H02M), C03V(H03V), C02D(H02D), C04A(H04A), C031(H031), C03O(H03O),
 C02Y(H02Y), C01V(H01V), C04D(H04D), C02Z(H02Z), C02L(H02L), C037(H037),
 C01Q(H01Q), C026(H026), C03H(H03H), C025(H025), C03N(H03N), C04B(H04B),
 C02W(H02W), C04R(H04R), C04O(H04O), C04P(H04P), C02I(H02I), C020(H020),
 C03Q(H03Q), C02S(H02S), C027(H027), C01T(H01T), C04U(H04U), C71(H71),
 C04M(H04M), C02V(H02V), C023(H023), C02X(H02X), C03J(H03J), C03W(H03W),
 C04E(H04E), C03R(H03R), C02G(H02G), C04H(H04H), C046(H046), C041(H041),
 C04G(H04G), C04Q(H04Q), C03K(H03K), C01S(H01S), C032(H032), C62(H62),
 C04L(H04L), C04I(H04I), C47(H47), C29(H29), C044(H044), C03F(H03F), C039(H039),
  C49(H49), C15(H15), C25(H25), C80(H80), C03E(H03E), C03L(H03L), C45(H45)
4.b Fitted hexagon refined as free rotating group:
 C01I(C01O,C02J,C01X,C03U,C02P), C01K(C02N,C029,C033,C035,C022), C01L(C03G,
 C042,C030,C02H,C01J), C01N(C01M,C03M,C04T,C045,C021), C01R(C036,C04C,C02M,C03V,
 C02D), C01W(C04A,C031,C03O,C02Y,C01V), C01Z(C04D,C02Z,C02L,C037,C01Q),
 C028(C049,C026,C03H,C025,C024), C02B(C040,C03N,C04B,C02W,C03S), C02K(C04R,C04O,
 C04P,C02I,C020), C02O(C01U,C03Q,C02S,C027,C02T), C02Q(C02E,C01T,C04U,C71,C04M),
  C02U(C02C,C03D,C02V,C023,C02X), C034(C04K,C03J,C03W,C04E,C03C), C03A(C03R,
 C02G,C04H,C046,C041), C03B(C03Z,C04G,C04Q,C03K,C02R), C03P(C01S,C032,C62,C04L,
 C04I), C03T(C47,C29,C044,C03F,C039), C047(C49,C15,C25,C80,C26), C048(C03Y,C03E,
 C03L,C45,C04J)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41918
_shelx_fab_checksum              89983
_olex2_submission_special_instructions 'No special instructions were received'