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_4347389
_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
'C76 H52 Co4 N32 6+, 6(B F4 -), C2 H3 N, 0.5(O)'
_chemical_formula_sum            'C78 H55 B6 Co4 F24 N33 O0.5'
_chemical_formula_weight         2219.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.046(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5051(6)
_cell_length_b                   23.2553(6)
_cell_length_c                   29.4800(12)
_cell_measurement_reflns_used    63498
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.722
_cell_measurement_theta_min      1.385
_cell_volume                     8551.7(6)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.1175
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            63498
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.722
_diffrn_reflns_theta_max         24.722
_diffrn_reflns_theta_min         1.385
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.9098
_exptl_absorpt_correction_T_min  0.7605
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_description       block
_exptl_crystal_F_000             4448
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1331
_refine_ls_number_reflns         14385
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0966
_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^)+(0.0134P)^2^+132.3302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2244
_refine_ls_wR_factor_ref         0.2331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11509
_reflns_number_total             14385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00106_si_002.cif
_cod_data_source_block           jin26_3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C78 H55 B6 Co4 F24 N33 O0.50'
_cod_database_code               4347389
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              50911
_shelx_hkl_checksum              71107