Transformations of empty Cu core to CuCuO and CuS cores <i>via</i> oxide and sulfide insertions.
Fukuda, Yosuke; Yoshinari, Nobuto; Yamagami, Kohei; Konno, Takumi; Chemical communications (Cambridge, England) 57 (2021) 5386–5389; doi:10.1039/d1cc01572a

data_7128250
_publ_section_title
;
 Transformations of empty Cu core to CuCuO and CuS cores <i>via</i> oxide
 and sulfide insertions.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5386
_journal_page_last               5389
_journal_paper_doi               10.1039/d1cc01572a
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_sum            'C36 H60 Cu4 N12 Na8 O24 Rh4 S12'
_chemical_formula_weight         2279.40
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-04-19 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5649(2)
_cell_length_b                   23.5649(2)
_cell_length_c                   23.5649(2)
_cell_measurement_reflns_used    14513
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.2470
_cell_measurement_theta_min      1.9320
_cell_volume                     13085.70(19)
_computing_cell_refinement       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.75a (Rigaku OD, 2020)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Mercury 2020.1'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.7631
_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      9.00  61.00   0.50   35.00    --   -2.84  60.00 -73.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0078134000
_diffrn_orient_matrix_UB_12      -0.0099816000
_diffrn_orient_matrix_UB_13      0.0272931000
_diffrn_orient_matrix_UB_21      -0.0239811000
_diffrn_orient_matrix_UB_22      0.0137758000
_diffrn_orient_matrix_UB_23      0.0118918000
_diffrn_orient_matrix_UB_31      -0.0164284000
_diffrn_orient_matrix_UB_32      -0.0248420000
_diffrn_orient_matrix_UB_33      -0.0043718000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24032
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         30.7124
_diffrn_reflns_theta_min         1.9324
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.75a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 3388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         10371
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0871P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     0.670
_reflns_number_gt                8719
_reflns_number_total             10369
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01572a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7128250--7128252.cif.'
_cod_original_cell_volume        13085.7(3)
_cod_database_code               7128250
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.769
_shelx_estimated_absorpt_t_max   0.851
_oxdiff_exptl_absorpt_empirical_full_min 0.872
_oxdiff_exptl_absorpt_empirical_full_max 1.404
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01c1cc24e1fc81f52a0866b13c2f32c32e0010440cf
;
_diffrn_oxdiff_digest_hkl
;
017a67b3500cef306b4e6497a4b0ccaf786d35
;
_shelx_res_checksum              83323
_shelx_fab_checksum              64687