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_4347126
_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(C3 H7 N O), 4(Br -), 2(O)'
_chemical_formula_sum            'C104 H84 Br8 Fe4 N28 O6'
_chemical_formula_weight         2684.67
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_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            4
_cell_length_a                   20.1962(3)
_cell_length_b                   20.1962(3)
_cell_length_c                   25.0077(4)
_cell_measurement_reflns_used    60796
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.637
_cell_measurement_theta_min      1.296
_cell_volume                     10200.3(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 0.999
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60796
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.637
_diffrn_reflns_theta_min         1.296
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.763
_exptl_absorpt_correction_T_max  0.6896
_exptl_absorpt_correction_T_min  0.3235
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 4156 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         9608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0302P)^2^+3.8742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0526
_refine_ls_wR_factor_ref         0.0533
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                9172
_reflns_number_total             9608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02762_si_002.cif
_cod_data_source_block           1f-mst18
_cod_database_code               4347126
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.255
_shelx_estimated_absorpt_t_max   0.779
_shelx_res_checksum              4868
_shelx_hkl_checksum              22467