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_1549839
_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         'C52 H56 F6 Fe4 O4'
_chemical_formula_sum            'C52 H56 F6 Fe4 O4'
_chemical_formula_weight         1082.36
_chemical_name_common            neisc52
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d'
_symmetry_space_group_name_Hall  '-I 4bd 2'
_symmetry_space_group_name_H-M   'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_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            8
_cell_length_a                   15.5897(4)
_cell_length_b                   15.5897(4)
_cell_length_c                   45.3118(12)
_cell_measurement_reflns_used    12384
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      26.27
_cell_measurement_theta_min      3.41
_cell_volume                     11012.5(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -45.00  21.88   0.38   71.89    --  -10.30  89.00-109.00  176
  2  \w    -65.00  -9.90   0.38   71.89    --    9.12 -57.00  60.00  145
  3  \w    -26.00  28.34   0.38   71.89    --  -10.30 -99.00   0.00  143
  4  \w    -26.00  28.34   0.38   71.89    --  -10.30 -99.00 -30.00  143
  5  \w    -45.00  23.02   0.38   71.89    --  -10.30 -89.00 134.00  179
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0187652000
_diffrn_orient_matrix_UB_12      0.0105634000
_diffrn_orient_matrix_UB_13      0.0137977000
_diffrn_orient_matrix_UB_21      -0.0051165000
_diffrn_orient_matrix_UB_22      -0.0442342000
_diffrn_orient_matrix_UB_23      0.0031856000
_diffrn_orient_matrix_UB_31      0.0411290000
_diffrn_orient_matrix_UB_32      -0.0006998000
_diffrn_orient_matrix_UB_33      0.0066837000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            39711
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.372
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.218
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3041
_refine_ls_number_restraints     204
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1130P)^2^+21.1445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2358
_reflns_number_total             3041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02915f2.cif
_cod_data_source_block           2d
_cod_original_cell_volume        11012.5(6)
_cod_database_code               1549839
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.876
_shelx_res_checksum              36527
_shelx_fab_checksum              97662