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_4347124
_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
;
 2(C92 H56 Br4 Fe4 N24 4+), 2(C4 H10 O2), 
 8(Cl O4 -), 0.5(C3 H7 N O)
;
_chemical_formula_sum            'C193.5 H135.5 Br8 Cl8 Fe8 N48.5 O36.5'
_chemical_formula_weight         5093.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                77.211(2)
_cell_angle_beta                 88.923(2)
_cell_angle_gamma                86.843(2)
_cell_formula_units_Z            2
_cell_length_a                   19.2517(5)
_cell_length_b                   20.2665(6)
_cell_length_c                   28.5810(8)
_cell_measurement_reflns_used    116379
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      24.645
_cell_measurement_theta_min      1.125
_cell_volume                     10857.9(5)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0956
_diffrn_reflns_av_unetI/netI     0.0839
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            116379
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.645
_diffrn_reflns_theta_max         24.645
_diffrn_reflns_theta_min         1.125
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.170
_exptl_absorpt_correction_T_max  0.8785
_exptl_absorpt_correction_T_min  0.3935
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             5104
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.110
_platon_squeeze_details
;
TITL mst31 in P-1
CELL   19.2517   20.2665   28.5810     77.21     88.92     86.84
SPGR P-1
C101 0.761 0.175 0.377 !       4.08 eA-3
C102 0.891 0.127 0.441 !       3.77 eA-3
C103 0.530 0.081 0.489 !       3.66 eA-3
C104 0.253 0.718 0.439 !       3.55 eA-3
C105 0.516 0.565 0.448 !       3.49 eA-3
C106 0.011 0.910 0.020 !       3.43 eA-3
C107 0.847 0.201 0.422 !       3.35 eA-3
C108 0.734 0.164 0.372 !       3.30 eA-3
Q109 0.295 0.643 0.300 !       3.07 eA-3
C110 0.771 0.170 0.427 !       2.96 eA-3
C111 0.278 0.719 0.386 !       2.95 eA-3
Q112 0.575 0.936 0.438 !       2.84 eA-3
C113 0.485 0.621 0.429 !       2.74 eA-3
C114 0.253 0.693 0.416 !       2.64 eA-3
C115 0.029 0.107-0.002 !       2.61 eA-3
C116 0.490 0.937 0.435 !       2.49 eA-3
C117 0.531 0.918 0.448 !       2.47 eA-3
C118 0.488 0.527 0.491 !       2.39 eA-3
C119 0.308 0.737 0.441 !       2.37 eA-3
C120 0.513 0.921 0.480 !       2.35 eA-3
C121 0.186 0.874 0.135 !       2.30 eA-3
C122 0.279 0.733 0.077 !       2.29 eA-3
C123 0.471 0.097 0.482 !       2.25 eA-3
C124 0.950 0.157 0.435 !       2.21 eA-3
C125 0.917 0.190 0.421 !       2.18 eA-3
C126 0.508 0.099 0.433 !       2.16 eA-3
C127 0.234 0.768 0.093 !       2.15 eA-3
C128 0.173 0.810 0.108 !       2.08 eA-3
C129 0.313 0.563 0.433 !       2.07 eA-3
C130 0.128 0.893 0.104 !       1.98 eA-3
C131 0.278 0.627 0.044 !       1.93 eA-3
C132 0.594 0.079 0.496 !       1.93 eA-3
C133 0.258 0.673 0.383 !       1.93 eA-3
Q134 0.564 0.943 0.474 !       1.89 eA-3
C135 0.223 0.701 0.067 !       1.88 eA-3
C136 0.163 0.866 0.120 !       1.86 eA-3
C137 0.461 0.094 0.443 !       1.77 eA-3
C138 0.343 0.496 0.449 !       1.75 eA-3
C139 0.375 0.483 0.455 !       1.75 eA-3
C140 0.223 0.642 0.048 !       1.74 eA-3
C141 0.137 0.876 0.152 !       1.70 eA-3
C142 0.303 0.607 0.391 !       1.69 eA-3
C143 0.111 0.753 0.129 !       1.65 eA-3
Q144 0.291 0.685 0.342 !       1.59 eA-3
Q145 0.142 0.738 0.187 !       1.58 eA-3
C146 0.387 0.516 0.432 !       1.56 eA-3
Q147 0.423 0.593 0.306 !       1.51 eA-3
Q148 0.515 0.467 0.243 !       1.51 eA-3
C149 0.266 0.785 0.452 !       1.51 eA-3
C150 0.330 0.749 0.469 !       1.51 eA-3
C151 0.430 0.941 0.470 !       1.48 eA-3
C152 0.290 0.675 0.080 !       1.48 eA-3
C153 0.425 0.545 0.443 !       1.47 eA-3
Q154 0.712 0.966 0.447 !       1.45 eA-3
C155 0.115 0.916 0.066 !       1.42 eA-3
Q156 0.137 0.652 0.018 !       1.40 eA-3
C157 0.283 0.764 0.418 !       1.38 eA-3
C158 0.205 0.670 0.443 !       1.37 eA-3
C159 0.233 0.757 0.460 !       1.36 eA-3
Q160 0.246 0.027 0.092 !       1.35 eA-3
Q161 0.172 0.620 0.180 !       1.34 eA-3
C162 0.409 0.529 0.458 !       1.34 eA-3
C163 0.487 0.470 0.489 !       1.33 eA-3
C164 0.441 0.627 0.421 !       1.31 eA-3
C165 0.067 0.854 0.156 !       1.29 eA-3
C166 0.217 0.779 0.447 !       1.29 eA-3
Q167 0.143 0.736 0.062 !       1.29 eA-3
C168 0.219 0.791 0.118 !       1.29 eA-3
C169 0.564 0.064 0.461 !       1.28 eA-3
Q170 0.732 0.123 0.398 !       1.27 eA-3
C171 0.964 0.892 0.065 !       1.27 eA-3
C172 0.471 0.506 0.475 !       1.27 eA-3
C173 0.235 0.674 0.452 !       1.23 eA-3
Q174 0.284 0.578 0.324 !       1.23 eA-3
C175 0.591 0.109 0.450 !       1.23 eA-3
C176 0.154 0.763 0.126 !       1.21 eA-3
Q177 0.563 0.440 0.210 !       1.20 eA-3
C178 0.011 0.908 0.061 !       1.20 eA-3
C179 0.059 0.842 0.027 !       1.20 eA-3
Q180 0.561 0.231 0.413 !       1.19 eA-3
C181 0.046 0.932 0.055 !       1.18 eA-3
Q182 0.279 0.264 0.025 !       1.17 eA-3
C183 0.954 0.072 0.025 !       1.17 eA-3
Q184 0.991 0.563 0.015 !       1.15 eA-3
Q185 0.152 0.715 0.079 !       1.14 eA-3
Q186 0.348 0.653 0.316 !       1.14 eA-3
C187 0.061 0.955 0.014 !       1.13 eA-3
C188 0.123 0.752 0.094 !       1.12 eA-3
C189 0.263 0.700 0.108 !       1.12 eA-3
C190 0.142 0.813 0.141 !       1.12 eA-3
C191 0.064 0.876 0.115 !       1.11 eA-3
Q192 0.591 0.968 0.462 !       1.11 eA-3
C193 0.375 0.563 0.435 !       1.11 eA-3
Q194 0.248 0.205 0.052 !       1.11 eA-3
Q195 0.893 0.330 0.038 !       1.11 eA-3
Q196 0.024 0.362 0.023 !       1.10 eA-3
C197 0.249 0.639 0.429 !       1.10 eA-3
C198 0.408 0.469 0.489 !       1.10 eA-3
Q199 0.586 0.964 0.489 !       1.09 eA-3
;
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2685
_refine_ls_number_reflns         36471
_refine_ls_number_restraints     466
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0919
_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^)+(0.1122P)^2^+39.2470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2180
_refine_ls_wR_factor_ref         0.2414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23851
_reflns_number_total             36471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02762_si_002.cif
_cod_data_source_block           1d-mst31_sq
_cod_original_formula_sum        'C193.50 H135.50 Br8 Cl8 Fe8 N48.50 O36.50'
_cod_database_code               4347124
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.410
_shelx_estimated_absorpt_t_max   0.796
_shelx_res_checksum              5550
_shelx_hkl_checksum              98368
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              5434