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_7128252
_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_moiety         'C36 H60 Cu6 N12 Na3 O36 Rh4 S13'
_chemical_formula_sum            'C36 H60 Cu6 N12 Na3 O36 Rh4 S13'
_chemical_formula_weight         2515.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.634(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6933(3)
_cell_length_b                   29.5973(4)
_cell_length_c                   15.8253(3)
_cell_measurement_reflns_used    4477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.45
_cell_measurement_theta_min      2.83
_cell_volume                     6389.1(2)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_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-2018 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type
'RIGAKU 1/4chi goniometer with PILATUS3 X CdTe 1M'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4126
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            261534
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.792
_diffrn_reflns_theta_full        14.333
_diffrn_reflns_theta_max         23.569
_diffrn_reflns_theta_min         1.479
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_correction_T_min  0.7439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       plate
_exptl_crystal_F_000             2486
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.840
_refine_diff_density_min         -1.630
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 16123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         77119
_refine_ls_number_restraints     1198
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.815
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.720
_reflns_number_gt                46950
_reflns_number_total             77119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc01572a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7128250--7128252.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7128252
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              69797
_shelx_fab_checksum              55195