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_7123249
_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 (C12 H11 Br N3)12 Br4],2 (C5 H11 N O) 2(C2 H6 O) 11(H2O)'
_chemical_formula_sum            'C158 H188 Br16 Co8 N38 O15'
_chemical_formula_weight         4609.42
_space_group_crystal_system      cubic
_space_group_IT_number           218
_space_group_name_Hall           'P -4n 2 3'
_space_group_name_H-M_alt        'P -4 3 n'
_symmetry_space_group_name_Hall  'P -4n 2 3'
_symmetry_space_group_name_H-M   'P -4 3 n'
_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            2
_cell_length_a                   21.5387(3)
_cell_length_b                   21.5387(3)
_cell_length_c                   21.5387(3)
_cell_measurement_reflns_used    1615
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.8637
_cell_measurement_theta_min      2.8990
_cell_volume                     9992.1(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4098
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.0801
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8052
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.834
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.018
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.192
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.59419
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            kermesinus
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       polyhedra
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 259 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.042(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2802
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1776
_refine_ls_R_factor_gt           0.0837
_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^)+(0.1463P)^2^+0.3006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2265
_refine_ls_wR_factor_ref         0.2850
_reflns_Friedel_coverage         0.564
_reflns_Friedel_fraction_full    0.682
_reflns_Friedel_fraction_max     0.659
_reflns_number_gt                1201
_reflns_number_total             2802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02083g2.cif
_cod_data_source_block           1a
_cod_original_cell_volume        9992.1(4)
_cod_database_code               7123249
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              85539
_shelx_fab_checksum              7189