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_4347387
_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 4+, 4(B F4 -), 2(C2 H3 N)'
_chemical_formula_sum            'C80 H58 B4 Co4 F16 N34'
_chemical_formula_weight         2078.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.6570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0340(3)
_cell_length_b                   13.3498(2)
_cell_length_c                   50.7076(9)
_cell_measurement_reflns_used    94032
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.598
_cell_measurement_theta_min      1.456
_cell_volume                     9468.8(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0683
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            94032
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.598
_diffrn_reflns_theta_max         24.598
_diffrn_reflns_theta_min         1.456
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.250
_platon_squeeze_details
;
TITL jin13     P 21/c       R = 0.10
CELL   14.0300   13.3520   50.7180     90.00     94.69     90.00
SPGR P21/c
C101 0.475 0.698 0.975 !       3.59 eA-3
C102 0.652 0.692 0.243 !       3.19 eA-3
C103 0.551 0.397 0.009 !       3.17 eA-3
C104 0.670 0.031 0.012 !       3.11 eA-3
C105 0.275 0.265 0.768 !       2.83 eA-3
C106 0.551 0.786 0.485 !       2.67 eA-3
C107 0.623 0.741 0.997 !       2.56 eA-3
C108 0.873 0.550 0.454 !       2.53 eA-3
C109 0.217 0.224 0.779 !       2.27 eA-3
C110 0.254 0.978 0.991 !       2.24 eA-3
C111 0.591 0.032 0.013 !       2.21 eA-3
C112 0.901 0.464 0.462 !       1.85 eA-3
C113 0.038 0.876 0.028 !       1.79 eA-3
C114 0.704 0.928 0.008 !       1.77 eA-3
C115 0.702 0.841 0.007 !       1.70 eA-3
C116 0.691 0.045 0.992 !       0.82 eA-3
Q117 0.609 0.410 0.739 !       0.78 eA-3
Q118 0.610 0.515 0.709 !       0.72 eA-3
C119 0.979 0.882-0.000 !       0.67 eA-3
C120 0.060 0.297 0.474 !       0.65 eA-3
Q121 0.029 0.039 0.914 !       0.65 eA-3
Q122 0.044 0.081 0.916 !       0.65 eA-3
Q123 0.100 0.864 0.637 !       0.59 eA-3
C124 0.078 0.172 0.986 !       0.55 eA-3
Q125 0.355 0.809 0.133 !       0.53 eA-3
Q126 0.575 0.327 0.376 !       0.52 eA-3
Q127 0.168 0.012 0.241 !       0.51 eA-3
Q128 0.228 0.846 0.461 !       0.50 eA-3
Q129 0.131 0.455 0.773 !       0.50 eA-3
;
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         15875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0875P)^2^+6.8352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1444
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12748
_reflns_number_total             15875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00106_si_002.cif
_cod_data_source_block           jin13_sq_1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347387
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.828
_shelx_res_checksum              34912
_shelx_hkl_checksum              63839
_shelx_fab_checksum              90581