Redox-Induced Single-Molecule Magnetism in Mixed-Valent [2 ×2] Co4 Grid Complexes.
Tong, Jin; Demeshko, Serhiy; John, Michael; Dechert, Sebastian; Meyer, Franc; Inorganic chemistry 55 (2016) 4362–4372; doi:10.1021/acs.inorgchem.6b00106

data_4347390
_publ_section_title
;
 Redox-Induced Single-Molecule Magnetism in Mixed-Valent [2 \\times 2] Co4
 Grid Complexes.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4362
_journal_page_last               4372
_journal_paper_doi               10.1021/acs.inorgchem.6b00106
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C80 H60 Co4 N32 6+, 6(B F4 -)'
_chemical_formula_sum            'C80 H60 B6 Co4 F24 N32'
_chemical_formula_weight         2226.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7367(4)
_cell_length_b                   24.7367(4)
_cell_length_c                   36.3344(7)
_cell_measurement_reflns_used    128964
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.705
_cell_measurement_theta_min      1.616
_cell_volume                     22233.2(7)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            128964
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.705
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             8944
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.192
_platon_squeeze_details
;
TITL jin25_a.res in I4(1)/acd
CELL   24.7367   24.7367   36.3344     90.00     90.00     90.00
SPGR I41/acd
C101 1.000 0.935 0.126 !       3.95 eA-3
C102 0.969 0.565 0.143 !       3.79 eA-3
C103 0.163 0.675 0.087 !       3.13 eA-3
C104 0.149 0.511 0.078 !       3.09 eA-3
C105 0.767 0.016 0.126 !       3.02 eA-3
C106 0.794 0.500 0.250 !       2.90 eA-3
C107 0.244 0.929 0.155 !       2.29 eA-3
C108 0.500 0.249 0.133 !       2.15 eA-3
C109 0.267 0.431 0.197 !       1.90 eA-3
C110 0.280 0.032 0.026 !       1.89 eA-3
C111 0.970 0.772 0.118 !       1.37 eA-3
C112 0.086 0.742 0.124 !       1.29 eA-3
Q113 0.939 0.187 0.126 !       0.83 eA-3
Q114 0.335 0.428 0.062 !       0.76 eA-3
C115 0.615 0.460 0.109 !       0.75 eA-3
Q116 0.194 0.707 0.085 !       0.75 eA-3
Q117 0.576 0.575 0.181 !       0.65 eA-3
Q118 0.491 0.751 0.196 !       0.63 eA-3
Q119 0.937 0.538 0.218 !       0.61 eA-3
Q120 0.795 0.846 0.170 !       0.59 eA-3
Q121 0.984 0.229 0.211 !       0.58 eA-3
Q122 0.906 0.177 0.139 !       0.58 eA-3
Q123 0.907 0.176 0.109 !       0.58 eA-3
C124 0.062 0.543 0.120 !       0.55 eA-3
Q125 0.086 0.191 0.228 !       0.55 eA-3
Q126 0.361 0.899 0.220 !       0.54 eA-3
Q127 0.483 0.610 0.116 !       0.52 eA-3
Q128 0.434 0.888 0.079 !       0.50 eA-3
;
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5275
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+81.4888P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4742
_reflns_number_total             5275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00106_si_002.cif
_cod_data_source_block           jin25_sq_4
_cod_original_cell_volume        22233.2(8)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4347390
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              63622
_shelx_hkl_checksum              34634
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              73071