Multinuclear Iron-Phenyl Species in Reactions of Simple Iron Salts and PhMgBr: Identification of Fe4(μ-Ph)6(THF)4 as a Key Reactive Species for Cross-Coupling
Carpenter, Stephanie H.; Baker, Tessa M.; Munoz, Salvador; Brennessel, William W.; Neidig, Michael L.; Chemical Science  (2018) –; doi:10.1039/C8SC02915F

data_1549841
_publ_section_title
;
 Multinuclear Iron-Phenyl Species in Reactions of Simple Iron Salts and
 PhMgBr: Identification of Fe4(\m-Ph)6(THF)4 as a Key Reactive Species for
 Cross-Coupling
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC02915F
_journal_year                    2018
_chemical_formula_moiety         'C30 H54 Mg N6 O6, C36 H30 Fe2, 3.5(C4 H8 O)'
_chemical_formula_sum            'C80 H112 Fe2 Mg N6 O9.5'
_chemical_formula_weight         1445.76
_chemical_name_common            neisc24
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.048(2)
_cell_length_b                   20.048(2)
_cell_length_c                   19.320(2)
_cell_measurement_reflns_used    4028
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.34
_cell_volume                     7765.1(14)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            78802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.272
_diffrn_reflns_theta_min         1.436
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             3096
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         7037
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0662P)^2^+6.4809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4657
_reflns_number_total             7037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02915f2.cif
_cod_data_source_block           1b
_cod_original_cell_volume        7764.9(18)
_cod_database_code               1549841
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              35277