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_7129536
_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 H66 Ag3 Cu2 S6, 2(C H2 Cl2), C19 H18 P'
_chemical_formula_sum            'C57 H88 Ag3 Cl4 Cu2 P S6'
_chemical_formula_weight         1589.09
_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                74.687(3)
_cell_angle_beta                 84.949(2)
_cell_angle_gamma                72.840(3)
_cell_formula_units_Z            2
_cell_length_a                   13.8063(4)
_cell_length_b                   14.8132(5)
_cell_length_c                   18.4926(6)
_cell_measurement_reflns_used    8990
_cell_measurement_temperature    190.00(10)
_cell_measurement_theta_max      27.8390
_cell_measurement_theta_min      2.5290
_cell_volume                     3485.2(2)
_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      190.00(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 0.831
_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    -36.00  31.00   1.00    5.00    --   15.65 -57.00 -60.00   67
  2  \w    -16.00  20.00   1.00    5.00    --  -16.43 -99.00  60.00   36
  3  \w     -4.00  49.00   1.00    5.00    --   15.65  37.00  90.00   53
  4  \w     -1.00  78.00   1.00    5.00    --   15.65  57.00 -90.00   79
  5  \w    -10.00  16.00   1.00    5.00    --  -16.43  77.00-180.00   26
  6  \w    -83.00 -10.00   1.00    5.00    --  -16.43 -77.00-180.00   73
  7  \w      4.00  82.00   1.00    5.00    --   15.65  57.00 120.00   78
;
_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      0.0200745000
_diffrn_orient_matrix_UB_12      0.0369836000
_diffrn_orient_matrix_UB_13      0.0046591000
_diffrn_orient_matrix_UB_21      -0.0015366000
_diffrn_orient_matrix_UB_22      -0.0183040000
_diffrn_orient_matrix_UB_23      0.0394801000
_diffrn_orient_matrix_UB_31      0.0498606000
_diffrn_orient_matrix_UB_32      -0.0312456000
_diffrn_orient_matrix_UB_33      -0.0011304000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32492
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.492
_diffrn_reflns_theta_min         1.910
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78712
_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    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         16131
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0628P)^2^+4.2927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1298
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11440
_reflns_number_total             16131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05135k2.cif
_cod_data_source_block           2076939
_cod_depositor_comments
'Adding full bibliography for 7129533--7129538.cif.'
_cod_database_code               7129536
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C58H90Ag3Cu2S6P1Cl6
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(Cl4) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(C56)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C17) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31)
2.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),
  C21(H21A,H21B), C22(H22A,H22B), 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),
  C56(H56A,H56B), C57(H57A,H57B)
2.c Aromatic/amide H refined with riding coordinates:
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46),
 C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
2.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19345
_shelx_hkl_checksum              90019
_shelx_fab_checksum              51637
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.891