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_7129534
_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         'C36 H64 Ag3 Cu2 S6, C H2 Cl2, C21 H22 P'
_chemical_formula_sum            'C58 H88 Ag3 Cl2 Cu2 P S6'
_chemical_formula_weight         1530.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 95.858(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0658(5)
_cell_length_b                   23.5120(11)
_cell_length_c                   20.5437(9)
_cell_measurement_reflns_used    8287
_cell_measurement_temperature    190.01(10)
_cell_measurement_theta_max      27.2160
_cell_measurement_theta_min      2.0870
_cell_volume                     6758.6(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.838
_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      0.00  60.00   1.00   15.00    --   15.65   0.00   0.00   60
  2  \w      3.00  75.00   1.00   15.00    --   15.65  57.00  90.00   72
  3  \w    -23.00  18.00   1.00   15.00    --  -16.43 -99.00-120.00   41
  4  \w    -54.00 -28.00   1.00   15.00    --   15.65   0.00   0.00   26
  5  \w      0.00  26.00   1.00   15.00    --   15.65  57.00-150.00   26
  6  \w    -33.00  44.00   1.00   15.00    --  -16.43  57.00-150.00   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      0.0012316000
_diffrn_orient_matrix_UB_12      -0.0301287000
_diffrn_orient_matrix_UB_13      0.0017335000
_diffrn_orient_matrix_UB_21      0.0039498000
_diffrn_orient_matrix_UB_22      0.0015105000
_diffrn_orient_matrix_UB_23      0.0346481000
_diffrn_orient_matrix_UB_31      -0.0505241000
_diffrn_orient_matrix_UB_32      -0.0006144000
_diffrn_orient_matrix_UB_33      -0.0008022000
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45165
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.586
_diffrn_reflns_theta_min         1.998
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77519
_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    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             3120
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.723
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         15919
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0747P)^2^+18.5154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10147
_reflns_number_total             15919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05135k2.cif
_cod_data_source_block           2076940
_cod_depositor_comments
'Adding full bibliography for 7129533--7129538.cif.'
_cod_database_code               7129534
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.534
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C19-C24 = C24-C23
 1.54 with sigma of 0.02
 C19-C23
 2.515 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C58(H58A,H58B), C37(H37A,H37B),
  C38(H38A,H38B)
3.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45),
 C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55),
  C56(H56), C57(H57)
3.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              42966
_shelx_hkl_checksum              24543
_shelx_fab_checksum              51623
_olex2_date_sample_data_collection 2021-04-02
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.762