Structural properties of [Cu(II)3L6] cages: bridged polyatomic anion effects on unprecedented efficiency of heterogeneous catechol oxidation
Kim, Doheon; Gwak, Geonwoo; Han, Jihun; Kim, Dongwon; Jung, Ok-Sang; Dalton Transactions  (2022) –; doi:10.1039/D2DT00500J

data_7709805
_publ_section_title
;
 Structural properties of [Cu(II)3L6] cages: bridged polyatomic anion
 effects on unprecedented efficiency of heterogeneous catechol oxidation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00500J
_journal_year                    2022
_chemical_formula_moiety
'6(C26 H32 Cu F5 N4 Si2.83), 2(Cl O4), 12(C H4 O)'
_chemical_formula_sum            'C168 H240 Cl2 Cu6 F30 N24 O20 Si17'
_chemical_formula_weight         4415.50
_space_group_crystal_system      cubic
_space_group_IT_number           195
_space_group_name_Hall           'P 2 2 3'
_space_group_name_H-M_alt        'P 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/2
_audit_update_record
;
2022-03-15 deposited with the CCDC.	2022-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.901(3)
_cell_length_b                   22.901(3)
_cell_length_c                   22.901(3)
_cell_measurement_reflns_used    184567
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.417
_cell_measurement_theta_min      0.435
_cell_volume                     12011(3)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program (Shin et. al, 2016)'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.760
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78859
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.988
_diffrn_reflns_theta_max         26.988
_diffrn_reflns_theta_min         1.345
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             4584
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 1433 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.041(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         7161
_refine_ls_number_restraints     605
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1661P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2581
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3878
_reflns_number_total             7161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00500j2.cif
_cod_data_source_block           CuClO4_a_sq
_cod_original_cell_volume        12011(4)
_cod_database_code               7709805
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.860
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              6218
_shelx_fab_checksum              7208