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_4347123
_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(F6 P -), 4(C3 H7 N O)'
_chemical_formula_sum            'C104 H84 Br4 F24 Fe4 N28 O4 P4'
_chemical_formula_weight         2912.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.2950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1679(2)
_cell_length_b                   27.6422(6)
_cell_length_c                   28.2611(4)
_cell_measurement_reflns_used    101202
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      25.669
_cell_measurement_theta_min      1.441
_cell_volume                     11067.8(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 0.987
_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  0.0859
_diffrn_reflns_av_unetI/netI     0.0994
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            101202
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.669
_diffrn_reflns_theta_min         1.441
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_T_max  0.9124
_exptl_absorpt_correction_T_min  0.5610
_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             5824
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.062(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3120
_refine_ls_number_reflns         40880
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0513P)^2^+1.3798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1303
_reflns_Friedel_coverage         0.959
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                30564
_reflns_number_total             40880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02762_si_002.cif
_cod_data_source_block           1b-mst36
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4347123
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.417
_shelx_estimated_absorpt_t_max   0.883
_shelx_res_checksum              12937
_shelx_hkl_checksum              55816