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_4347388
_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 4+, 4(B F4 -)'
_chemical_formula_sum            'C80 H60 B4 Co4 F16 N32'
_chemical_formula_weight         2052.56
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2359(3)
_cell_length_b                   17.2359(3)
_cell_length_c                   13.2617(2)
_cell_measurement_reflns_used    47837
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.631
_cell_measurement_theta_min      1.671
_cell_volume                     3939.74(11)
_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-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.631
_diffrn_reflns_theta_min         1.671
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.9273
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'yellow brown'
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0376P)^2^+2.3396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3418
_reflns_number_total             3712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00106_si_002.cif
_cod_data_source_block           jin15_2
_cod_original_cell_volume        3939.74(15)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4347388
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.912
_shelxl_version_number           2013-4
_shelx_res_checksum              97649
_shelx_hkl_checksum              43338