Isolation, Characterization, and Reactivity of Fe8Me12(-): Kochi's S = 1/2 Species in Iron-Catalyzed Cross-Couplings with MeMgBr and Ferric Salts.
Muñoz Iii, Salvador B; Daifuku, Stephanie L.; Brennessel, William W.; Neidig, Michael L.; Journal of the American Chemical Society 138 (2016) 7492–7495; doi:10.1021/jacs.6b03760

data_4130463
_publ_section_title
;
 Isolation, Characterization, and Reactivity of Fe8Me12(-): Kochi's S =
 1/2 Species in Iron-Catalyzed Cross-Couplings with MeMgBr and Ferric
 Salts.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7492
_journal_page_last               7495
_journal_paper_doi               10.1021/jacs.6b03760
_journal_volume                  138
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety
; 
 C20 H40 Br0.082 Cl0.918 Mg O5, C12 H36 Fe8, 
 0.5(C16 H32 Br0.334 Cl1.666 Mg O4), 3(C4 H8 O) 
;
_chemical_formula_sum            'C52 H116 Br0.25 Cl1.75 Fe8 Mg1.5 O10'
_chemical_formula_weight         1466.72
_chemical_name_common            neism18h
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_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                   38.445(4)
_cell_length_b                   13.0221(14)
_cell_length_c                   13.6580(15)
_cell_measurement_reflns_used    4072
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.22
_cell_volume                     6837.7(13)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            92013
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.922
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015a)'
_exptl_crystal_colour            yellow-black
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             3090
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         15680
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0996P)^2^+1.1895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12489
_reflns_number_total             15680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b03760_si_002.cif
_cod_data_source_block           neism18h
_cod_original_cell_volume        6837.6(13)
_cod_original_formula_sum        'C52 H116 Br0.25 Cl1.75 Fe8 Mg1.50 O10'
_cod_database_code               4130463
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.635
_shelx_estimated_absorpt_t_max   0.802
_shelx_res_checksum              44208
_shelx_hkl_checksum              93221