Control over synthesis of homovalent and mixed-valent cubic cobalt-imidazolate cages
Liang, Liang; Luo, Dong; Zuo, Tao; Zhou, Xiao-Ping; Li, Dan; Chemical Communications  (2019) –; doi:10.1039/C9CC02083G

data_7123251
_publ_section_title
;
 Control over synthesis of homovalent and mixed-valent cubic
 cobalt-imidazolate cages
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02083G
_journal_year                    2019
_chemical_formula_moiety
'[Co8 (C13 H11 F3 N3)12 Br4],2 (Co Br4) Br 8(C3 H7 N O) 9.625(C4 H10 O) 2.125(H2O)'
_chemical_formula_sum            'C218.5 H132 Br13 Co10 F36 N44 O19.75'
_chemical_formula_weight         6001.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-12 deposited with the CCDC.    2019-04-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0922(19)
_cell_length_b                   30.1286(12)
_cell_length_c                   68.447(3)
_cell_measurement_reflns_used    3759
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.4620
_cell_measurement_theta_min      3.8780
_cell_volume                     49683(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1109
_diffrn_reflns_av_unetI/netI     0.1434
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -78
_diffrn_reflns_number            31574
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.829
_diffrn_reflns_theta_min         3.890
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.142
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.41724
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            kermesinus
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             18952
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.514
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         12276
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.2629
_refine_ls_R_factor_gt           0.1405
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3732
_refine_ls_wR_factor_ref         0.4544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4731
_reflns_number_total             12276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02083g2.cif
_cod_data_source_block           4
_cod_database_code               7123251
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              13115
_shelx_fab_checksum              34907