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_1549835
_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         'C36 H30 Fe2, 2(C21 H39 Mg O6), 4(C4 H8 O)'
_chemical_formula_sum            'C94 H140 Fe2 Mg2 O16'
_chemical_formula_weight         1686.37
_chemical_name_common            neisc21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-06-25 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                69.5966(19)
_cell_angle_beta                 81.444(2)
_cell_angle_gamma                88.910(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4649(12)
_cell_length_b                   12.9212(12)
_cell_length_c                   15.2879(15)
_cell_measurement_reflns_used    4074
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      24.58
_cell_measurement_theta_min      2.32
_cell_volume                     2280.7(4)
_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-2016/4 (Sheldrick, 2016b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_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  0.1039
_diffrn_reflns_av_unetI/netI     0.1137
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.481
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         1.653
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         10437
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5850
_reflns_number_total             10437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02915f2.cif
_cod_data_source_block           1a
_cod_database_code               1549835
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              52278