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_7123250
_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 F N3)12 Br4], (C5 H11 N O) 2.5(C2 H6 O) 17.5(H2O)'
_chemical_formula_sum            'C154 H193 Br4 Co8 F12 N37 O21'
_chemical_formula_weight         3917.52
_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   mixed
_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                   21.0860(2)
_cell_length_b                   21.0860(2)
_cell_length_c                   21.0860(2)
_cell_measurement_reflns_used    5945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.1700
_cell_measurement_theta_min      4.6900
_cell_volume                     9375.24(15)
_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
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12346
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.854
_diffrn_reflns_theta_min         4.689
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_exptl_absorpt_coefficient_mu    6.911
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.36002
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            atrovirens
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             3444
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Flack x determined using 895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.040(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         3008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0619
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+16.2313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.694
_reflns_Friedel_fraction_full    0.841
_reflns_Friedel_fraction_max     0.802
_reflns_number_gt                2577
_reflns_number_total             3008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02083g2.cif
_cod_data_source_block           2
_cod_original_cell_volume        9375.2(3)
_cod_database_code               7123250
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              11750
_shelx_fab_checksum              93460