Magnetostructural Correlation for High-Nuclearity Iron(III)/Oxo Complexes and Application to Fe5, Fe6, and Fe8 Clusters.
Mitchell, Kylie J.; Abboud, Khalil A.; Christou, George; Inorganic chemistry 55 (2016) 6597–6608; doi:10.1021/acs.inorgchem.6b00769

data_4347913
_publ_section_title
;
 Magnetostructural Correlation for High-Nuclearity Iron(III)/Oxo Complexes
 and Application to Fe5, Fe6, and Fe8 Clusters.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6597
_journal_page_last               6608
_journal_paper_doi               10.1021/acs.inorgchem.6b00769
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C88 H64 N2 O26 Fe6, (2(CH2 Cl2)'
_chemical_formula_sum            'C90 H68 Cl4 Fe6 N2 O26'
_chemical_formula_weight         2070.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                   21.6936(13)
_cell_length_b                   17.4045(10)
_cell_length_c                   23.6770(14)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     8939.6(9)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2014 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1129
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            171215
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       plate
_exptl_crystal_F_000             4216
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         10282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0364P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6611
_reflns_number_total             10282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00769_si_001.cif
_cod_data_source_block           kjm41
_cod_database_code               4347913
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.808
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              29107
_shelx_hkl_checksum              73086