Serendipitous formation of oxygen-bridged CuII6M (M = MnII, CoII) double cubanes showing electrocatalytic water oxidation
San Esteban, Anna Carissa M.; Kuwamura, Naoto; Yoshinari, Nobuto; Konno, Takumi; Chemical Communications  (2022) –; doi:10.1039/D1CC07199H

data_7129780
_publ_section_title
;
 Serendipitous formation of oxygen-bridged CuII6M (M = MnII, CoII) double
 cubanes showing electrocatalytic water oxidation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC07199H
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C30 H60 Br2 Co Cu6 N6 O18 S6, 6(H2 O) [+ 14.5(H2O)]'
_chemical_formula_sum            'C30 H101 Br2 Co Cu6 N6 O38.5 S6'
_chemical_formula_weight         1954.51
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.0980(7)
_cell_length_b                   15.0980(7)
_cell_length_c                   55.4613(14)
_cell_measurement_reflns_used    133072
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.685
_cell_measurement_theta_min      0.645
_cell_volume                     10948.6(8)
_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
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'RIGAKU1/4chi goniometer with PILATUS3 X CdTe 1M'
_diffrn_measurement_method       /w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4148
_diffrn_reflns_av_R_equivalents  0.1200
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            176713
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.411
_diffrn_reflns_theta_max         15.625
_diffrn_reflns_theta_min         0.643
_diffrn_source                   'SPring-8 BL02B1 bending magnet'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8251
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             5988
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 11606 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.046(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1423
_refine_ls_number_reflns         33452
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                28513
_reflns_number_total             33452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc07199h2.cif
_cod_data_source_block           Co
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C60 H202 Br4 Co2 Cu12 N12 O77 S12'
_cod_original_formula_weight         3909.02
_cod_original_formula_moiety
'2(C30 H60 Br2 Co Cu6 N6 O18 S6), 12(H2 O) [+ 29(H2O)]'
_cod_original_formula_units_Z            3
_cod_original_cell_volume        10948.6(11)
_cod_database_code               7129780
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.928
_shelx_estimated_absorpt_t_max   0.928
_shelx_res_checksum              18413
_shelx_fab_checksum              83727