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_1569433
_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                   24.05180(10)
_cell_length_b                   24.08610(10)
_cell_length_c                   24.12200(10)
_cell_measurement_reflns_used    145752
_cell_measurement_temperature    150
_cell_measurement_theta_max      74.0820
_cell_measurement_theta_min      2.6160
_cell_volume                     13974.21(10)
_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 2013/2 (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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -57.00 -31.00   0.50    0.50    --    0.00 -19.00 150.00   52
  2  \w     53.00  86.00   0.50    0.50    --    0.00  77.00  30.00   66
  3  \w     55.00  88.00   0.50    0.50    --    0.00  77.00 -30.00   66
  4  \w    -68.00 -27.00   0.50    0.50    --    0.00 -57.00 -90.00   82
  5  \w    -77.00  18.00   0.50    0.50    --    0.00 -38.00 -60.00  190
  6  \w    -15.00  24.00   0.50    0.50    --    0.00 -19.00 150.00   78
  7  \w     11.00  37.00   0.50    0.50    --    0.00  77.00  30.00   52
  8  \w    -29.00  12.00   0.50    0.50    --    0.00  77.00 -30.00   82
  9  \w    -57.00  19.00   0.50    0.50    --    0.00 -38.00   0.00  152
 10  \w    -19.00  23.00   0.50    0.50    --    0.00 -57.00 -90.00   84
 11  \w    -30.00  -4.00   0.50    0.50    --    0.00  77.00  30.00   52
 12  \w    -89.00  22.00   0.50    0.50    --    0.00 -57.00-150.00  222
 13  \w    -87.00  23.00   0.50    0.50    --    0.00 -57.00 120.00  220
 14  \w     63.00  95.00   0.50    1.50    --   95.80  82.00  60.00   64
 15  \w     43.00 124.00   0.50    1.50    --   95.80 -82.00 -30.00  162
 16  \w    108.00 185.00   0.50    1.50    --   95.80  76.00 -10.95  154
 17  \w     70.00 185.00   0.50    1.50    --   95.80  63.00  38.82  230
 18  \w    138.00 184.00   0.50    1.50    --   95.80  78.00-112.01   92
 19  \w     65.00  90.00   0.50    1.50    --   95.80  76.00 -10.95   50
 20  \w    158.00 185.00   0.50    1.50    --   95.80  64.00-148.33   54
 21  \w     65.00  90.00   0.50    1.50    --   95.80  77.00-180.00   50
 22  \w     65.00  90.00   0.50    1.50    --   95.80  77.00 120.00   50
 23  \w     65.00  91.00   0.50    1.50    --   95.80  77.00-150.00   52
 24  \w     65.00  90.00   0.50    1.50    --   95.80  77.00-120.00   50
 25  \w      7.00 128.00   0.50    1.50    --   95.80 -82.00 120.00  242
 26  \w     63.00  88.00   0.50    1.50    --   95.80  82.00 -60.00   50
 27  \w     63.00 126.00   0.50    1.50    --   95.80  82.00   0.00  126
 28  \w    152.00 177.00   0.50    1.50    --   95.80  82.00   0.00   50
 29  \w     65.00  96.00   0.50    1.50    --   95.80  77.00  60.00   62
 30  \w    100.00 126.00   0.50    1.50    --   95.80  77.00  60.00   52
 31  \w     65.00  98.00   0.50    1.50    --   95.80  78.00-112.01   66
 32  \w     58.00 118.00   0.50    1.50    --   95.80 -82.00 -90.00  120
 33  \w     65.00  99.00   0.50    1.50    --   95.80  77.00  90.00   68
 34  \w     69.00  95.00   0.50    1.50    --   95.80  67.00 -29.99   52
 35  \w    107.00 184.00   0.50    1.50    --   95.80  68.00 -58.39  154
 36  \w     75.00 147.00   0.50    1.50    --   95.80  45.00 -60.00  144
 37  \w     83.00 127.00   0.50    1.50    --   95.80 -82.00-180.00   88
 38  \w    160.00 185.00   0.50    1.50    --   95.80  77.00 -90.00   50
 39  \w     75.00 161.00   0.50    1.50    --   95.80  45.00 120.00  172
 40  \w     65.00 103.00   0.50    1.50    --   95.80  77.00 150.00   76
 41  \w     63.00  88.00   0.50    1.50    --   95.80  82.00 -90.00   50
 42  \w     33.00  79.00   0.50    1.50    --   95.80 -82.00-180.00   92
 43  \w     75.00 182.00   0.50    1.50    --   95.80  45.00-150.00  214
 44  \w     65.00  90.00   0.50    1.50    --   95.80  77.00 -60.00   50
 45  \w     65.00  91.00   0.50    1.50    --   95.80  77.00  30.00   52
 46  \w    115.00 140.00   0.50    1.50    --   95.80  77.00  30.00   50
 47  \w     63.00  88.00   0.50    1.50    --   95.80  82.00-150.00   50
 48  \w     65.00  90.00   0.50    1.50    --   95.80  77.00 -30.00   50
 49  \w    159.00 184.00   0.50    1.50    --   95.80  77.00 -30.00   50
 50  \w    114.00 174.00   0.50    1.50    --   95.80  82.00  30.00  120
 51  \w     65.00  90.00   0.50    1.50    --   95.80  77.00 -90.00   50
 52  \w     63.00  89.00   0.50    1.50    --   95.80  82.00  90.00   52
 53  \w     63.00  97.00   0.50    1.50    --   95.80  82.00 150.00   68
 54  \w     75.00 100.00   0.50    1.50    --   95.80  45.00  90.00   50
 55  \w    123.00 185.00   0.50    1.50    --   95.80  45.00  90.00  124
 56  \w     75.00 101.00   0.50    1.50    --   95.80  45.00 150.00   52
 57  \w     75.00 106.00   0.50    1.50    --   95.80  45.00 -90.00   62
 58  \w    117.00 183.00   0.50    1.50    --   95.80  76.00 140.82  132
 59  \w     65.00  90.00   0.50    1.50    --   95.80  77.00   0.00   50
 60  \w     63.00  88.00   0.50    1.50    --   95.80  82.00-180.00   50
 61  \w    123.00 185.00   0.50    1.50    --   95.80  82.00-180.00  124
 62  \w     75.00 107.00   0.50    1.50    --   95.80  45.00-120.00   64
 63  \w     63.00  88.00   0.50    1.50    --   95.80  82.00  30.00   50
 64  \w     71.00 103.00   0.50    1.50    --   95.80  61.00   0.00   64
 65  \w    113.00 185.00   0.50    1.50    --   95.80  82.00 120.00  144
 66  \w     63.00  88.00   0.50    1.50    --   95.80  82.00 120.00   50
 67  \w    131.00 164.00   0.50    1.50    --   95.80  45.00-120.00   66
 68  \w    158.00 185.00   0.50    1.50    --   95.80  82.00  60.00   54
 69  \w     65.00  90.00   0.50    1.50    --   95.80  76.00 140.82   50
 70  \w     68.00  93.00   0.50    1.50    --   95.80  68.00 -58.39   50
 71  \w     70.00  95.00   0.50    1.50    --   95.80  64.00-148.33   50
 72  \w     46.00 128.00   0.50    1.50    --   95.80 -82.00  30.00  164
 73  \w     73.00 182.00   0.50    1.50    --   95.80  52.00 -33.11  218
;
_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      0.0317637000
_diffrn_orient_matrix_UB_12      -0.0278370000
_diffrn_orient_matrix_UB_13      -0.0479913000
_diffrn_orient_matrix_UB_21      0.0479323000
_diffrn_orient_matrix_UB_22      -0.0143994000
_diffrn_orient_matrix_UB_23      0.0398747000
_diffrn_orient_matrix_UB_31      -0.0282388000
_diffrn_orient_matrix_UB_32      -0.0557510000
_diffrn_orient_matrix_UB_33      0.0136048000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            351767
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.602
_diffrn_reflns_theta_min         2.592
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28171
_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    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             5680
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.999
_refine_diff_density_min         -1.244
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 12049 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.0088(18)
_refine_ls_extinction_coef       0.000018(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1424
_refine_ls_number_reflns         28438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+17.2730P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                27179
_reflns_number_total             28438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nr03095d2.cif
_cod_data_source_block           Ag6-R
_cod_depositor_comments
'Adding full bibliography for 1569433--1569435.cif.'
_cod_database_code               1569433
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O N  S Ag'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.590
_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:
 N14(H14), N5(H5), C126(H126), C55(H55), C57(H57), C53(H53), C96(H96),
 C109(H109), C35(H35), C120(H120), C40(H40), C32(H32), C44(H44), C49(H49),
 C36(H36), C51(H51), C58(H58), C72(H72), C114(H114), C52(H52), C26(H26),
 C60(H60), C33(H33), C99(H99), C34(H34), C22(H22), C101(H101), C125(H125),
 C107(H107), C85(H85), C6(H6), C20(H20), C9(H9), C76(H76), C63(H63), C98(H98),
 C92(H92), C62(H62), C73(H73), C100(H100), C118(H118), C70(H70), C23(H23),
 C86(H86), C38(H38), C68(H68), C59(H59), C28(H28), C102(H102), C71(H71),
 C83(H83), C24(H24), C88(H88), C8(H8), C78(H78), C30(H30), C29(H29), C80(H80),
 C81(H81), C124(H124), C117(H117), C116(H116), C103(H103), C46(H46), C61(H61),
 C4(H4), C69(H69), C48(H48), C27(H27), C90(H90), C122(H122), C87(H87), C82(H82),
  C111(H111), C93(H93), C43(H43), C12(H12), C41(H41), C89(H89), C47(H47),
 C110(H110), C11(H11), C75(H75), C94(H94), C16(H16), C123(H123), C42(H42),
 C64(H64), C19(H19), C65(H65), C105(H105), C104(H104), C13(H13), C115(H115),
 C18(H18), C17(H17), C95(H95), C10(H10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64960
_shelx_fab_checksum              4273
_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 2.650
_oxdiff_exptl_absorpt_empirical_full_min 0.746