Unlocking spontaneous chiral resolution in silver clusters through steric and anionic control.
Liu, Jin; Nan, Zi-Ang; Li, Qing; Shen, Chuan-Qi; Wang, Zuo-Bei; Lin, Fu-Lin; Chen, Ting; Liu, Lu-Yao; Xie, Zhuo-Zhou; Zhuo, Zhu; Wang, Wei; Huang, You-Gui; Chemical science 17 (2026) 4948–4954; doi:10.1039/d5sc08561f

data_1576527
_publ_section_title
;
 Unlocking spontaneous chiral resolution in silver clusters through steric
 and anionic control.
;
_journal_issue                   10
_journal_name_full               'Chemical science'
_journal_page_first              4948
_journal_page_last               4954
_journal_paper_doi               10.1039/d5sc08561f
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety
'C72.5 H54 Ag3 F1.5 N14 O1.5 S0.5, 2.5(C F3 O3 S)'
_chemical_formula_sum            'C75 H54 Ag3 F9 N14 O9 S3'
_chemical_formula_weight         1886.11
_space_group_crystal_system      cubic
_space_group_IT_number           212
_space_group_name_Hall           'P 4acd 2ab 3'
_space_group_name_H-M_alt        'P 43 3 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-12-23
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-12-25 deposited with the CCDC.	2026-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.18680(10)
_cell_length_b                   27.18680(10)
_cell_length_c                   27.18680(10)
_cell_measurement_reflns_used    340771
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.0070
_cell_measurement_theta_min      1.9240
_cell_volume                     20094.36(13)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -37.00  48.00   0.50    3.50    --   18.71 -89.00   0.00  170
  2  \w    -49.00  42.00   0.50    3.50    --  -20.12  89.00 116.00  182
  3  \w    -49.00  42.00   0.50    3.50    --  -20.12  89.00 116.00  182
  4  \w    -18.00  52.00   0.50    3.50    --   18.71 -99.00-120.00  140
  5  \w      3.00  94.00   0.50    3.50    --   18.71  19.00   0.00  182
  6  \w      4.00  92.00   0.50    3.50    --   18.71  38.00-180.00  176
  7  \w      4.00  92.00   0.50    3.50    --   18.71  38.00-180.00  176
  8  \w     -5.00  92.00   0.50    3.50    --   18.71  77.00 -60.00  194
  9  \w      3.00  94.00   0.50    3.50    --   18.71  19.00   0.00  182
 10  \w     -9.00  41.00   0.50    3.50    --   18.71  89.00 116.00  100
 11  \w    -93.00  -4.00   0.50    3.50    --  -20.12 -57.00-180.00  178
 12  \w    -94.00  -5.00   0.50    3.50    --  -20.12 -38.00-180.00  178
 13  \w    -77.00 -21.00   0.50    3.50    --  -20.12 139.00 117.30  112
 14  \w    -77.00 -21.00   0.50    3.50    --  -20.12 139.00-137.46  112
 15  \w    -94.00  -5.00   0.50    3.50    --  -20.12 -38.00   0.00  178
 16  \w    -75.00 -20.00   0.50    3.50    --  -20.12 136.00 -21.19  110
 17  \w    -77.00 -21.00   0.50    3.50    --  -20.12 139.00  11.83  112
 18  \w    -93.00   4.00   0.50    3.50    --  -20.12 -77.00  90.00  194
 19  \w    -93.00  -4.00   0.50    3.50    --  -20.12 -57.00 -30.00  178
 20  \w     -5.00  92.00   0.50    3.50    --   18.71  77.00  60.00  194
 21  \w    -78.00 -23.00   0.50    3.50    --  -20.12 142.00 173.72  110
 22  \w    -75.00 -20.00   0.50    3.50    --  -20.12 136.00 -58.56  110
 23  \w    -65.00 -11.00   0.50    3.50    --  -20.12 121.00  85.33  108
 24  \w    -92.00 -42.00   0.50    3.50    --  -20.12-178.00 -60.00  100
 25  \w    -77.00 -21.00   0.50    3.50    --  -20.12 139.00  92.07  112
 26  \w    -76.00 -21.00   0.50    3.50    --  -20.12 138.00  40.53  110
 27  \w    -75.00 -20.00   0.50    3.50    --  -20.12 136.00 -35.12  110
 28  \w    -77.00 -21.00   0.50    3.50    --  -20.12 139.00-100.97  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0066
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            1102911
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         1.835
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             7552
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.658
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7699
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1103P)^2^+40.8738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2061
_reflns_Friedel_coverage         0.741
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6901
_reflns_number_total             7699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc08561f2.cif
_cod_data_source_block           exp_9768_auto
_cod_depositor_comments
'Adding full bibliography for 1576523--1576527.cif.'
_cod_original_cell_volume        20094.4(2)
_cod_database_code               1576527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     NAIFEI-1
_cell_oxdiff_angle_alpha         89.9277(5)
_cell_oxdiff_angle_beta          90.0358(5)
_cell_oxdiff_angle_gamma         89.8860(5)
_cell_oxdiff_length_a            27.16907(18)
_cell_oxdiff_length_b            27.17421(17)
_cell_oxdiff_length_c            27.21726(18)
_cell_oxdiff_measurement_reflns_used 340396
_cell_oxdiff_volume              20094.4(2)
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(7)
 0.10(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Restrained distances
 C2-F3 = C2-F4 = C2-F5
 1.33 with sigma of 0.02
 C3-F1 = C3-F2 = C3-F6
 1.33 with sigma of 0.02
 C3-S1
 1.82 with sigma of 0.02
 C1-F22
 1.325 with sigma of 0.01
 S1-O1 = S1-O2 = S1-O3
 1.44 with sigma of 0.02
 F22-F22_$3
 2.12 with sigma of 0.02
 C2-S6
 1.82 with sigma of 0.02
 F1-F6
 2.132 with sigma of 0.02
 S6-O7 = S6-O8 = S6-O9
 1.44 with sigma of 0.02
 O13_$1-S2_$2
 1.612 with sigma of 0.02
 O13_$1-O13_$2
 2.571 with sigma of 0.02
 S2-F22
 2.591 with sigma of 0.02
 C1-S2
 1.785 with sigma of 0.02
 S2-O13
 1.44 with sigma of 0.02
 C3-O1
 2.58 with sigma of 0.04
 C3-O2
 2.56 with sigma of 0.04
 C3-O3
 2.57 with sigma of 0.04
 C2-O7
 2.58 with sigma of 0.04
 C2-O8
 2.56 with sigma of 0.04
 C2-O9
 2.57 with sigma of 0.04
 C3-F1 \\sim C3-F2 \\sim C3-F6
 with sigma of 0.02
 F1-F2 \\sim F2-F6 \\sim F6-F1
 with sigma of 0.04
 S1-F1 \\sim S1-F2 \\sim S1-F6
 with sigma of 0.04
 S1-O1 \\sim S1-O2 \\sim S1-O3
 with sigma of 0.02
 O1-O2 \\sim O2-O3 \\sim O1-O3
 with sigma of 0.04
 C3-O1 \\sim C3-O2 \\sim C3-O3
 with sigma of 0.04
 C2-F3 \\sim C2-F4 \\sim C2-F5
 with sigma of 0.02
 F3-F4 \\sim F4-F5 \\sim F5-F3
 with sigma of 0.04
 S6-F3 \\sim S6-F4 \\sim S6-F5
 with sigma of 0.04
 S6-O7 \\sim S6-O8 \\sim S6-O9
 with sigma of 0.02
 O7-O8 \\sim O8-O9 \\sim O7-O9
 with sigma of 0.04
 C2-O7 \\sim C2-O8 \\sim C2-O9
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
S1 \\sim C3 \\sim F1 \\sim F2 \\sim F6 \\sim O1 \\sim O2 \\sim O3: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
F5 \\sim C2 \\sim F3 \\sim F4 \\sim S6 \\sim O7 \\sim O8 \\sim O9: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F22 \\sim C1 \\sim S2 \\sim F22 \\sim F22 \\sim O13 \\sim O13 \\sim O13: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(S1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C2(0.5) F3(0.5) F4(0.5) F5(0.5) S6(0.5) O7(0.5) O8(0.5) O9(0.5)
 C1(0.166667) S2(0.166667) O13(0.5) F22(0.5) C3(0.333333) F1(0.333333)
 F2(0.333333) F6(0.333333) S1(0.333333) O1(0.333333) O2(0.333333) O3(0.333333)
6.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C00T(H00D,H00E)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N006(H006), C00C(H00C), C00F(H00F), C00K(H00K), C00N(H00N),
 C00Q(H00Q), C00S(H00S), C00U(H00U), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C00Z(H00Z), C011(H011)
;
_shelx_res_checksum              91728
_shelx_fab_checksum              72192
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.473
_oxdiff_exptl_absorpt_empirical_full_min 0.684