Atomically precise chiral silver clusters based on non-chiral ligands for acid/base stimulated luminescence response.
Wang, Shuaibo; He, Weimiao; Cui, Yujia; Zhou, Zhan; Ma, Lufang; Zang, Shuang-Quan; Nanoscale 15 (2023) 12679–12685; doi:10.1039/d3nr03095d

data_1569434
_publ_section_title
;
 Atomically precise chiral silver clusters based on non-chiral ligands for
 acid/base stimulated luminescence response.
;
_journal_issue                   30
_journal_name_full               Nanoscale
_journal_page_first              12679
_journal_page_last               12685
_journal_paper_doi               10.1039/d3nr03095d
_journal_volume                  15
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C124 H98 Ag6 N16 P8 S4'
_chemical_formula_sum            'C124 H98 Ag6 N16 P8 S4'
_chemical_formula_weight         2835.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-06
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-06 deposited with the CCDC.	2023-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.01420(10)
_cell_length_b                   24.14150(10)
_cell_length_c                   24.1607(2)
_cell_measurement_reflns_used    128369
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.4940
_cell_measurement_theta_min      2.6050
_cell_volume                     14006.90(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_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    -85.00  55.00   0.50    0.50    --    0.00 -17.00 -83.09  280
  2  \w    -85.00  -7.00   0.50    0.50    --    0.00 -57.00 120.00  156
  3  \w    -21.00   6.00   0.50    0.50    --    0.00  38.00   0.00   54
  4  \w    -86.00  29.00   0.50    0.50    --    0.00 -57.00-180.00  230
  5  \w    -37.00  37.00   0.50    0.50    --    0.00  82.00  30.00  148
  6  \w    -83.00 -40.00   0.50    0.50    --    0.00 -38.00 -90.00   86
  7  \w     50.00  87.00   0.50    0.50    --    0.00  82.00  30.00   74
  8  \w     32.00  72.00   0.50    0.50    --    0.00  38.00   0.00   80
  9  \w      1.00  28.00   0.50    0.50    --    0.00 -57.00 120.00   54
 10  \w     15.00  45.00   0.50    0.50    --    0.00  19.00-150.00   60
 11  \w    -89.00 -64.00   0.50    0.50    --    0.00 -57.00 -90.00   50
 12  \w     29.00  83.00   0.50    0.50    --    0.00  38.00-150.00  108
 13  \w    -40.00  25.00   0.50    0.50    --    0.00 -57.00 -90.00  130
 14  \w    -27.00  29.00   0.50    0.50    --    0.00 -38.00 -90.00  112
 15  \w    -43.00   0.00   0.50    0.50    --    0.00  19.00-150.00   86
 16  \w    -28.00  -3.00   0.50    0.50    --    0.00  38.00-150.00   50
 17  \w    129.00 169.00   0.50    1.50    --   98.80  80.00 -22.41   80
 18  \w     61.00  87.00   0.50    1.50    --   98.80  80.00 -22.41   52
 19  \w    130.00 187.00   0.50    1.50    --   98.80  61.00 133.21  114
 20  \w     98.00 187.00   0.50    1.50    --   98.80  80.00 -80.68  178
 21  \w     61.00  87.00   0.50    1.50    --   98.80  82.00-150.00   52
 22  \w     61.00  90.00   0.50    1.50    --   98.80  80.00 -80.68   58
 23  \w     68.00  99.00   0.50    1.50    --   98.80  61.00 133.21   62
 24  \w     63.00  88.00   0.50    1.50    --   98.80  77.00  90.00   50
 25  \w     61.00  86.00   0.50    1.50    --   98.80  82.00 120.00   50
 26  \w    112.00 188.00   0.50    1.50    --   98.80  82.00 120.00  152
 27  \w    159.00 185.00   0.50    1.50    --   98.80  40.00 149.34   52
 28  \w     63.00  89.00   0.50    1.50    --   98.80  77.00 -90.00   52
 29  \w     61.00  92.00   0.50    1.50    --   98.80  82.00 150.00   62
 30  \w      9.00  70.00   0.50    1.50    --   98.80 -82.00-180.00  122
 31  \w     11.00 136.00   0.50    1.50    --   98.80 -82.00 -90.00  250
 32  \w     82.00 136.00   0.50    1.50    --   98.80 -82.00 120.00  108
 33  \w    150.00 187.00   0.50    1.50    --   98.80  81.00  10.63   74
 34  \w     38.00  77.00   0.50    1.50    --   98.80 -82.00 120.00   78
 35  \w    137.00 163.00   0.50    1.50    --   98.80  82.00  60.00   52
 36  \w     61.00 129.00   0.50    1.50    --   98.80  81.00  10.63  136
 37  \w    139.00 165.00   0.50    1.50    --   98.80  71.00-177.42   52
 38  \w     71.00 188.00   0.50    1.50    --   98.80  45.00  90.00  234
 39  \w     61.00  87.00   0.50    1.50    --   98.80  82.00 -60.00   52
 40  \w     70.00 156.00   0.50    1.50    --   98.80  45.00 120.00  172
 41  \w     63.00  88.00   0.50    1.50    --   98.80  77.00 150.00   50
 42  \w     70.00 187.00   0.50    1.50    --   98.80  45.00-150.00  234
 43  \w     61.00  86.00   0.50    1.50    --   98.80  82.00-120.00   50
 44  \w     61.00  87.00   0.50    1.50    --   98.80  82.00  90.00   52
 45  \w    153.00 186.00   0.50    1.50    --   98.80  82.00  90.00   66
 46  \w     63.00  89.00   0.50    1.50    --   98.80  77.00 120.00   52
 47  \w     63.00  89.00   0.50    1.50    --   98.80  77.00 -30.00   52
 48  \w     61.00  86.00   0.50    1.50    --   98.80  82.00  60.00   50
 49  \w     63.00  88.00   0.50    1.50    --   98.80  77.00  60.00   50
 50  \w     63.00  88.00   0.50    1.50    --   98.80  77.00 -60.00   50
 51  \w     70.00 188.00   0.50    1.50    --   98.80  45.00   0.00  236
 52  \w     63.00  89.00   0.50    1.50    --   98.80  77.00-150.00   52
 53  \w    158.00 188.00   0.50    1.50    --   98.80  77.00-150.00   60
 54  \w     61.00  86.00   0.50    1.50    --   98.80  82.00   0.00   50
 55  \w     63.00  89.00   0.50    1.50    --   98.80  77.00   0.00   52
 56  \w    163.00 188.00   0.50    1.50    --   98.80  77.00-120.00   50
 57  \w     61.00 108.00   0.50    1.50    --   98.80  80.00  35.96   94
 58  \w     63.00  88.00   0.50    1.50    --   98.80  77.00  30.00   50
 59  \w     70.00 156.00   0.50    1.50    --   98.80  55.00 -38.22  172
 60  \w     63.00  88.00   0.50    1.50    --   98.80  77.00-120.00   50
 61  \w    123.00 182.00   0.50    1.50    --   98.80  82.00-180.00  118
 62  \w    133.00 170.00   0.50    1.50    --   98.80  67.00 -85.47   74
 63  \w     68.00  97.00   0.50    1.50    --   98.80  61.00-120.00   58
 64  \w     72.00 168.00   0.50    1.50    --   98.80  45.00  30.00  192
 65  \w     61.00  86.00   0.50    1.50    --   98.80  82.00-180.00   50
 66  \w     85.00 124.00   0.50    1.50    --   98.80 -82.00-180.00   78
 67  \w    158.00 183.00   0.50    1.50    --   98.80  61.00-120.00   50
 68  \w     36.00 132.00   0.50    1.50    --   98.80 -82.00  30.00  192
 69  \w     70.00  96.00   0.50    1.50    --   98.80  45.00-180.00   52
 70  \w     66.00 125.00   0.50    1.50    --   98.80  67.00 -85.47  118
 71  \w     47.00 129.00   0.50    1.50    --   98.80 -82.00 -60.00  164
 72  \w     66.00 132.00   0.50    1.50    --   98.80 -82.00  90.00  132
 73  \w     70.00 182.00   0.50    1.50    --   98.80  52.00-129.33  224
 74  \w     65.00  93.00   0.50    1.50    --   98.80  71.00-177.42   56
 75  \w     69.00 126.00   0.50    1.50    --   98.80  40.00 149.34  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0132937000
_diffrn_orient_matrix_UB_12      0.0612577000
_diffrn_orient_matrix_UB_13      -0.0120131000
_diffrn_orient_matrix_UB_21      -0.0626469000
_diffrn_orient_matrix_UB_22      -0.0137079000
_diffrn_orient_matrix_UB_23      -0.0011756000
_diffrn_orient_matrix_UB_31      -0.0037165000
_diffrn_orient_matrix_UB_32      0.0115220000
_diffrn_orient_matrix_UB_33      0.0626057000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            339360
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.775
_diffrn_reflns_theta_min         2.587
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.399
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             5680
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.460
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Flack x determined using 11327 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(2)
_refine_ls_extinction_coef       0.000031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         28183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0776P)^2^+16.6043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                26285
_reflns_number_total             28183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03095d2.cif
_cod_data_source_block           Ag6-S
_cod_depositor_comments
'Adding full bibliography for 1569433--1569435.cif.'
_cod_database_code               1569434
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.553
_shelx_estimated_absorpt_t_min   0.432
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C72(H72), N12(H12), C70(H70), C82(H82), C111(H111), C86(H86), N4(H4),
 C58(H58), C104(H104), C85(H85), C15(H15), C124(H124), C102(H102), C69(H69),
 C89(H89), C62(H62), C18(H18), C47(H47), C16(H16), C88(H88), C67(H67), C87(H87),
  C103(H103), C57(H57), C34(H34), C83(H83), C96(H96), C49(H49), C37(H37),
 C5(H5), C116(H116), C1(H1), C17(H17), C13(H13), C8(H8), C66(H66), C109(H109),
 C29(H29), C10(H10), C94(H94), C36(H36), C22(H22), C73(H73), C4(H4A), C21(H21),
 C120(H120), C107(H107), C93(H93), C78(H78), C12(H12A), C19(H19), C51(H51),
 C84(H84), C9(H9), C77(H77), C53(H53), C68(H68), C121(H121), C92(H92),
 C123(H123), C24(H24), C65(H65), C39(H39), C28(H28), C52(H52), C7(H7), C55(H55),
  C114(H114), C33(H33), C56(H56), C3(H3), C60(H60), C2(H2), C46(H46), C23(H23),
 C118(H118), C31(H31), C40(H40), C99(H99), C43(H43), C50(H50), C25(H25),
 C63(H63), C100(H100), C80(H80), C75(H75), C108(H108), C122(H122), C41(H41),
 C64(H64), C79(H79), C45(H45), C32(H32), C27(H27), C74(H74), C44(H44), C38(H38),
  C26(H26)
;
_shelx_res_checksum              46983
_shelx_fab_checksum              82694
_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 9.038
_oxdiff_exptl_absorpt_empirical_full_min 0.448