Alloying and dealloying of Au<sub>18</sub>Cu<sub>32</sub> nanoclusters at precise locations <i>via</i> controlling the electronegativity of substituent groups on thiol ligands.
Tang, Li; Wang, Bin; Wang, Ru; Wang, Shuxin; Nanoscale 15 (2023) 1602–1608; doi:10.1039/d2nr05401a

data_1568236
_publ_section_title
;
 Alloying and dealloying of Au<sub>18</sub>Cu<sub>32</sub> nanoclusters at
 precise locations <i>via</i> controlling the electronegativity of
 substituent groups on thiol ligands.
;
_journal_issue                   4
_journal_name_full               Nanoscale
_journal_page_first              1602
_journal_page_last               1608
_journal_paper_doi               10.1039/d2nr05401a
_journal_volume                  15
_journal_year                    2023
_chemical_formula_moiety
'C215.983 H71.994 Au17.999 Cu31.997 F65.995 S35.997'
_chemical_formula_sum            'C216 H72 Au18 Cu32 F66 S36'
_chemical_formula_weight         10653.57
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      cubic
_space_group_IT_number           226
_space_group_name_Hall           '-F 4a 2 3'
_space_group_name_H-M_alt        'F m -3 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-23
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2021-12-23 deposited with the CCDC.	2022-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   42.573(5)
_cell_length_b                   42.573(5)
_cell_length_c                   42.573(5)
_cell_measurement_reflns_used    105236
_cell_measurement_temperature    120
_cell_measurement_theta_max      70.04
_cell_measurement_theta_min      6.23
_cell_volume                     77162(16)
_computing_cell_refinement       'X-Area Recipe 1.34.0.0 (STOE, 2019)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.161.0 (STOE, 2020)'
_computing_data_reduction
;
X-Area Integrate 1.78.0.0 (STOE, 2020)
X-Area LANA 1.78.0.0 (STOE, 2020)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      '1664 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  0.0748
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            124367
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.715
_diffrn_reflns_theta_min         6.150
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    16.697
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5976
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             39104
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.291
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3179
_refine_ls_number_restraints     675
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0554
_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^)+(0.1362P)^2^+232.5677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2294
_reflns_number_total             3179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nr05401a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1568236--1568237.cif.'
_cod_original_cell_volume        77161(28)
_cod_original_sg_symbol_Hall     '-F 4c 2 3'
_cod_database_code               1568236
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.286
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C16-C11 = C15-C16 = C15-C14 = C13-C14 = C13-C12 = C12-C11
 1.39 with sigma of 0.001
 C1-C2 = C2-C3 = C4-C3 = C5-C4 = C5-C6 = C6-C1
 1.39 with sigma of 0.001
 C5-C4
 1.39 with sigma of 0.001
 F2-C4
 1.35 with sigma of 0.02
 F2-C3
 2.4 with sigma of 0.02
 C1-C10 = C10-C9 = C4-C9 = C8-C4 = C7-C8 = C1-C7
 1.39 with sigma of 0.001
 C8-C10
 2.78 with sigma of 0.001
 C9-C7
 2.78 with sigma of 0.001
 C5-F3
 1.35 with sigma of 0.03
 F3-C5
 1.34 with sigma of 0.01
 F1-C9
 1.35 with sigma of 0.02
 C4-C9 \\sim C10-C9 \\sim C1-C10 \\sim C1-C7 \\sim C7-C8 \\sim C8-C4
 with sigma of 0.02
 C4-F3 \\sim F3-C6
 with sigma of 0.02
 C5-F2 \\sim F2-C3
 with sigma of 0.02
 C4-F1 \\sim F1-C10
 with sigma of 0.02
3. Restrained planarity
 C12, C13, C14, C15, C16, C11
 with sigma of 0.1
 C1, C4, C2, C3, C5, C6
 with sigma of 0.1
 F4, F5, C12, C13, C14, C15, C16, S2, C11
 with sigma of 0.1
 S1, F2, F3, C1, C4, C2, C3, C5, C6
 with sigma of 0.1
 C1, C4, C7, C8, C9, C10
 with sigma of 0.1
 F1, C1, C4, C7, C8, C9, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim C1 \\sim C4 \\sim C12 \\sim C13
\\sim C14 \\sim C15 \\sim C16 \\sim C2 \\sim C3 \\sim C5 \\sim C6 \\sim C11
\\sim C7 \\sim C8 \\sim C9 \\sim C10: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 3.8A
S1 \\sim F1 \\sim F2 \\sim F3 \\sim C1 \\sim C4 \\sim C2 \\sim C3 \\sim C5
\\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
F4 \\sim F5 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim S2 \\sim
C11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Others
 Fixed Sof: F1(0.5) F3(0.25) F4(0.5) F5(0.5) C6(0.5) H6(0.5) C5(0.5) C3(0.5)
 H3(0.5) C2(0.5) H2(0.5) S2(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5) C15(0.5)
 C16(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) C10(0.5) H10(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C2(H2), C7(H7), C8(H8), C10(H10)
6.b Fitted hexagon refined as free rotating group:
 C1(C6,C5,C4,C3,C2), C11(C12,C13,C14,C15,C16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54086
_shelx_fab_checksum              34829
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'