Controllable spontaneous resolution in ultrasmall Cu-Ag bimetallic cluster ion pairs from achiral components.
He, Jiao; Deng, Cheng-Long; Sun, Cun-Fa; Zhang, Xiao-Xiao; Cui, Ying; Wu, Sheng-Hui; Luo, Geng-Geng; Chemical communications (Cambridge, England) 58 (2022) 1577–1580; doi:10.1039/d1cc05135k

data_7129535
_publ_section_title
;
 Controllable spontaneous resolution in ultrasmall Cu-Ag bimetallic
 cluster ion pairs from achiral components.
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1577
_journal_page_last               1580
_journal_paper_doi               10.1039/d1cc05135k
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C24 H54 Ag3 Cu2 S6, C24 H20 P'
_chemical_formula_sum            'C48 H74 Ag3 Cu2 P S6'
_chemical_formula_weight         1325.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-18 deposited with the CCDC.	2021-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                103.801(4)
_cell_angle_beta                 93.205(4)
_cell_angle_gamma                97.260(4)
_cell_formula_units_Z            2
_cell_length_a                   12.5420(7)
_cell_length_b                   12.5516(7)
_cell_length_c                   19.3067(10)
_cell_measurement_reflns_used    8918
_cell_measurement_temperature    190.01(10)
_cell_measurement_theta_max      28.8020
_cell_measurement_theta_min      2.3950
_cell_volume                     2916.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      190.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0606
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.836
_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    -49.00  32.00   1.00   10.00    --   15.49 -57.00 -90.00   81
  2  \w     -6.00  54.00   1.00   10.00    --   15.49 -99.00   0.00   60
  3  \w    -21.00  23.00   1.00   10.00    --  -16.28 -99.00-180.00   44
  4  \w    -23.00  50.00   1.00   10.00    --  -16.28  38.00-180.00   73
  5  \w    -25.00  51.00   1.00   10.00    --  -16.28  77.00  30.00   76
  6  \w     -1.00  76.00   1.00   10.00    --   15.49  57.00 120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0371819000
_diffrn_orient_matrix_UB_12      0.0120077000
_diffrn_orient_matrix_UB_13      -0.0251393000
_diffrn_orient_matrix_UB_21      0.0020659000
_diffrn_orient_matrix_UB_22      -0.0523624000
_diffrn_orient_matrix_UB_23      -0.0236111000
_diffrn_orient_matrix_UB_31      -0.0434700000
_diffrn_orient_matrix_UB_32      -0.0239159000
_diffrn_orient_matrix_UB_33      0.0159128000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27325
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.481
_diffrn_reflns_theta_min         2.226
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.978
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.850
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         13552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0703P)^2^+7.1404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1415
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10152
_reflns_number_total             13552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05135k2.cif
_cod_data_source_block           2076941
_cod_depositor_comments
'Adding full bibliography for 7129533--7129538.cif.'
_cod_database_code               7129535
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
1.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              48215
_shelx_hkl_checksum              31541
_shelx_fab_checksum              96084
_olex2_date_sample_data_collection 2021-03-24
_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 1.252
_oxdiff_exptl_absorpt_empirical_full_min 0.862