Spin-State Versatility in a Series of Fe4 [2 × 2] Grid Complexes: Effects of Counteranions, Lattice Solvent, and Intramolecular Cooperativity.
Steinert, Markus; Schneider, Benjamin; Dechert, Sebastian; Demeshko, Serhiy; Meyer, Franc; Inorganic chemistry 55 (2016) 2363–2373; doi:10.1021/acs.inorgchem.5b02762

data_4347125
_publ_section_title
;
 Spin-State Versatility in a Series of Fe4 [2 \\times 2] Grid Complexes:
 Effects of Counteranions, Lattice Solvent, and Intramolecular
 Cooperativity.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2363
_journal_page_last               2373
_journal_paper_doi               10.1021/acs.inorgchem.5b02762
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C92 H56 Br4 Fe4 N24 4+, 4(B F4 -)'
_chemical_formula_sum            'C92 H56 B4 Br4 F16 Fe4 N24'
_chemical_formula_weight         2387.88
_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                   24.1748(5)
_cell_length_b                   24.1748(5)
_cell_length_c                   45.7058(11)
_cell_measurement_reflns_used    72818
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.680
_cell_measurement_theta_min      1.488
_cell_volume                     26711.4(10)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1112
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            72818
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.680
_diffrn_reflns_theta_max         24.680
_diffrn_reflns_theta_min         1.488
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.688
_exptl_absorpt_correction_T_max  0.5844
_exptl_absorpt_correction_T_min  0.4952
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             9472
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.360
_platon_squeeze_details
;
TITL mst29c in I4(1)/acd
CELL   24.1748   24.1748   45.7058     90.00     90.00     90.00
SPGR I41/acd
C101 0.529 0.005 0.020 !       2.17 eA-3
C102 0.476 0.997 0.023 !       2.08 eA-3
C103 0.987 0.230 0.071 !       1.58 eA-3
C104 0.487 0.730 0.571 !       1.58 eA-3
C105 0.495 0.714 0.070 !       1.53 eA-3
C106 0.012 0.273 0.684 !       1.51 eA-3
C107 0.521 0.699 0.084 !       1.33 eA-3
C108 0.502 0.796 0.170 !       1.32 eA-3
Q109 0.087 0.783 0.231 !       1.25 eA-3
C110 0.683 0.597 0.055 !       1.25 eA-3
C111 0.819 0.133 0.059 !       1.19 eA-3
C112 0.345 0.876 0.072 !       1.12 eA-3
C113 0.118 0.412 0.209 !       1.10 eA-3
C114 0.811 0.094 0.140 !       1.08 eA-3
C115 0.300 0.860 0.036 !       1.07 eA-3
C116 0.658 0.578 0.172 !       1.07 eA-3
C117 0.189 0.393 0.081 !       1.07 eA-3
C118 0.823 0.126 0.019 !       1.05 eA-3
C119 0.321 0.939 0.153 !       1.05 eA-3
C120 0.318 0.959 0.127 !       1.05 eA-3
C121 0.826 0.078 0.124 !       1.04 eA-3
C122 0.855 0.106 0.054 !       1.04 eA-3
C123 0.215 0.385 0.047 !       1.03 eA-3
C124 0.348 0.874 0.184 !       1.01 eA-3
C125 0.477 0.815 0.158 !       1.01 eA-3
C126 0.372 0.929 0.157 !       0.99 eA-3
C127 0.372 0.570 0.656 !       0.99 eA-3
C128 0.156 0.439 0.058 !       0.99 eA-3
C129 0.656 0.594 0.125 !       0.99 eA-3
C130 0.362 0.951 0.132 !       0.98 eA-3
C131 0.373 0.966 0.247 !       0.98 eA-3
C132 0.873 0.466 0.747 !       0.98 eA-3
C133 0.707 0.604 0.031 !       0.98 eA-3
C134 0.721 0.122 0.995 !       0.98 eA-3
C135 0.849 0.096 0.222 !       0.98 eA-3
C136 0.709 0.615 0.071 !       0.97 eA-3
C137 0.868 0.101 0.115 !       0.97 eA-3
C138 0.638 0.529 0.229 !       0.97 eA-3
C139 0.365 0.892 0.089 !       0.97 eA-3
C140 0.193 0.897 0.006 !       0.95 eA-3
C141 0.676 0.110 0.897 !       0.95 eA-3
C142 0.684 0.546 0.229 !       0.94 eA-3
C143 0.188 0.500 0.250 !       0.93 eA-3
C144 0.814 0.040 0.246 !       0.93 eA-3
C145 0.301 0.932 0.043 !       0.92 eA-3
C146 0.731 0.500 0.250 !       0.91 eA-3
C147 0.471 0.705 0.158 !       0.91 eA-3
C148 0.784 0.012 0.235 !       0.89 eA-3
C149 0.319 0.007 0.239 !       0.88 eA-3
C150 0.469 0.792 0.054 !       0.86 eA-3
C151 0.585 0.570 0.211 !       0.86 eA-3
C152 0.208 0.429 0.075 !       0.86 eA-3
C153 0.838 0.037 0.158 !       0.85 eA-3
C154 0.312 0.890 0.165 !       0.84 eA-3
C155 0.123 0.624 0.461 !       0.83 eA-3
C156 0.377 0.876 0.039 !       0.83 eA-3
C157 0.189 0.454 0.059 !       0.83 eA-3
C158 0.665 0.556 0.081 !       0.82 eA-3
C159 0.537 0.692 0.098 !       0.80 eA-3
C160 0.385 0.906 0.142 !       0.79 eA-3
C161 0.325 0.937 0.023 !       0.78 eA-3
C162 0.636 0.365 0.469 !       0.77 eA-3
C163 0.690 0.619 0.217 !       0.76 eA-3
C164 0.251 0.859 0.001 !       0.72 eA-3
C165 0.401 0.943 0.239 !       0.71 eA-3
C166 0.670 0.068-0.001 !       0.70 eA-3
C167 0.656 0.101 0.013 !       0.69 eA-3
C168 0.800 0.124 0.179 !       0.69 eA-3
C169 0.504 0.200 0.354 !       0.67 eA-3
C170 1.004 0.700 0.854 !       0.67 eA-3
C171 0.996 0.300 0.146 !       0.67 eA-3
C172 0.507 0.803 0.104 !       0.67 eA-3
C173 0.370 0.830 0.044 !       0.67 eA-3
C174 0.503 0.297 0.866 !       0.67 eA-3
C175 0.406 0.959 0.192 !       0.66 eA-3
Q176 0.937 0.876 0.149 !       0.66 eA-3
Q177 0.508 0.824 0.009 !       0.65 eA-3
C178 0.363 0.970 0.102 !       0.65 eA-3
C179 0.971 0.237 0.135 !       0.64 eA-3
C180 0.765 0.054 0.033 !       0.64 eA-3
Q181 0.416 0.139 0.118 !       0.63 eA-3
C182 0.306 0.960 0.084 !       0.62 eA-3
C183 0.302 0.867 0.191 !       0.60 eA-3
C184 0.392 0.866 0.071 !       0.60 eA-3
C185 0.561 0.677 0.084 !       0.60 eA-3
C186 0.289 0.318 0.241 !       0.60 eA-3
C187 0.450 0.751 0.043 !       0.58 eA-3
C188 0.640 0.477 0.224 !       0.57 eA-3
C189 0.500 0.750 0.141 !       0.56 eA-3
C190 0.530 0.655 0.091 !       0.56 eA-3
C191 0.337 0.858 0.149 !       0.55 eA-3
C192 0.337 0.360 0.852 !       0.55 eA-3
C193 0.217 0.519 0.227 !       0.55 eA-3
C194 0.438 0.842 0.074 !       0.53 eA-3
C195 0.409 0.947 0.036 !       0.53 eA-3
C196 0.549 0.697 0.125 !       0.52 eA-3
C197 0.402 0.938 0.144 !       0.51 eA-3
Q198 0.957 0.658 0.006 !       0.51 eA-3
C199 0.909 0.173 0.200 !       0.51 eA-3
;
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         5644
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0812
_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^)+(0.0859P)^2^+35.3497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1805
_refine_ls_wR_factor_ref         0.1963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3894
_reflns_number_total             5644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02762_si_002.cif
_cod_data_source_block           1e-mst29c_sq
_cod_original_cell_volume        26711.4(13)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4347125
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.582
_shelx_res_checksum              23644
_shelx_hkl_checksum              38110
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              6355