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_7129533
_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, C H2 Cl2, C20 H20 P'
_chemical_formula_sum            'C57 H88 Ag3 Cl2 Cu2 P S6'
_chemical_formula_weight         1518.19
_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                 96.203(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1108(5)
_cell_length_b                   23.2804(12)
_cell_length_c                   20.4826(10)
_cell_measurement_reflns_used    7252
_cell_measurement_temperature    190.00(10)
_cell_measurement_theta_max      28.2130
_cell_measurement_theta_min      2.4130
_cell_volume                     6689.2(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      190.00(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 0.838
_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    -47.00  45.00   1.00   15.00    --   15.65 -19.00  60.00   92
  2  \w    -12.00  23.00   1.00   15.00    --  -16.43 -99.00  30.00   35
  3  \w    -25.00   0.00   1.00   15.00    --  -16.43 -99.00-120.00   25
  4  \w      3.00  47.00   1.00   15.00    --  -16.43  37.00-150.00   44
  5  \w    -36.00 -10.00   1.00   15.00    --  -16.43  37.00-150.00   26
  6  \w     50.00  87.00   1.00   15.00    --   15.65 178.00 -60.00   37
;
_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      -0.0041422000
_diffrn_orient_matrix_UB_12      -0.0303442000
_diffrn_orient_matrix_UB_13      -0.0016993000
_diffrn_orient_matrix_UB_21      -0.0254979000
_diffrn_orient_matrix_UB_22      0.0023840000
_diffrn_orient_matrix_UB_23      -0.0316468000
_diffrn_orient_matrix_UB_31      0.0434996000
_diffrn_orient_matrix_UB_32      -0.0014891000
_diffrn_orient_matrix_UB_33      -0.0143801000
_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  0.0394
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.838
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38176
_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         29.573
_diffrn_reflns_theta_min         2.000
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61991
_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    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.148
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         15726
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0644
_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^)+(0.0792P)^2^+17.6801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10285
_reflns_number_total             15726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05135k2.cif
_cod_data_source_block           2076933
_cod_depositor_comments
'Adding full bibliography for 7129533--7129538.cif.'
_cod_database_code               7129533
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ag3Cu2S6PCl4C58H85
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 C2-C3 = C3-C4
 1.54 with sigma of 0.02
 C1-C2 = C2-C3
 1.54 with sigma of 0.02
 C4-C5 = C5-C6
 1.54 with sigma of 0.02
 C3-C4 = C4-C5
 1.54 with sigma of 0.02
 C7-C12 = C12-C11
 1.54 with sigma of 0.02
 C5-C6 = C6-C1
 1.54 with sigma of 0.02
 C7-C12A = C12A-C11A
 1.54 with sigma of 0.02
 C12A-C7
 1.52 with sigma of 0.02
 C4-C6
 2.515 with sigma of 0.04
 C7-C11
 2.515 with sigma of 0.04
 C3-C5
 2.515 with sigma of 0.04
 C5-C1
 2.515 with sigma of 0.04
 C1-C3
 2.515 with sigma of 0.04
 C2-C4
 2.515 with sigma of 0.04
 C7-C11A
 2.515 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(Cl1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(Cl2) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 1-FVAR(1)
 Sof(H7A)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=
 Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=
 Sof(H12D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7B), C7(H7A), C13(H13), C19(H19), C25(H25), C31(H31)
4.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),
 C8A(H8AA,H8AB), C9(H9A,H9B), C9A(H9AA,H9AB), C10(H10A,H10B), C10A(H10C,H10D),
 C11(H11A,H11B), C11A(H11C,H11D), C12(H12A,H12B), C12A(H12C,H12D), 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), C57(H57A,H57B), C37(H37A,H37B)
4.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47),
 C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
4.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95752
_shelx_hkl_checksum              4080
_shelx_fab_checksum              92854
_olex2_date_sample_data_collection 2021-03-02
_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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.691