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_7123252
_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 H14 N3)12 Br4],3Br (N 03) (C5 H11 N O) 0.25(C2 H6 O) 1.625(H2O)'
_chemical_formula_sum            'C166.5 H194.1 Br7 Co8 N39 O3.9'
_chemical_formula_weight         3834.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 120.657(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.5517(18)
_cell_length_b                   19.0256(7)
_cell_length_c                   35.950(2)
_cell_measurement_reflns_used    14527
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6180
_cell_measurement_theta_min      2.8420
_cell_volume                     17976(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
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.936
_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  0.0576
_diffrn_reflns_av_unetI/netI     0.0540
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            37292
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.428
_diffrn_reflns_theta_min         2.867
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_exptl_absorpt_coefficient_mu    7.929
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.62863
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            atrovirens
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       block
_exptl_crystal_F_000             7756
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.275
_refine_diff_density_min         -3.448
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.483
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         18089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.483
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_gt           0.1238
_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          0.3519
_refine_ls_wR_factor_ref         0.3665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14125
_reflns_number_total             18089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02083g2.cif
_cod_data_source_block           3
_cod_database_code               7123252
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              59928
_shelx_fab_checksum              8094