Experimental and computational studies of the mechanism of iron-catalysed C‒H activation/functionalisation with allyl electrophiles
DeMuth, Joshua C.; Song, Zhihui; Carpenter, Stephanie H.; Boddie, Theresa E.; Radović, Aleksa; Baker, Tessa M.; Gutierrez, Osvaldo; Neidig, Michael L.; Chemical Science  (2021) –; doi:10.1039/D1SC01661J

data_1563604
_publ_section_title
;
 Experimental and computational studies of the mechanism of iron-catalysed
 C--H activation/functionalisation with allyl electrophiles
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC01661J
_journal_year                    2021
_chemical_formula_moiety         'C60 H49 Br Fe P4'
_chemical_formula_sum            'C60 H49 Br Fe P4'
_chemical_formula_weight         1029.63
_chemical_name_common            neisc20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-10-02 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                80.274(2)
_cell_angle_beta                 76.661(2)
_cell_angle_gamma                65.621(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8690(12)
_cell_length_b                   12.0085(14)
_cell_length_c                   20.318(2)
_cell_measurement_reflns_used    4073
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      23.77
_cell_measurement_theta_min      2.16
_cell_volume                     2342.1(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.1827
_diffrn_reflns_av_unetI/netI     0.1210
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            74820
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.315
_diffrn_reflns_theta_min         1.868
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       plate
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1209
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0536P)^2^+1.9446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5584
_reflns_number_total             8494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc01661j2.cif
_cod_data_source_block           neisc20
_cod_original_cell_volume        2342.2(5)
_cod_database_code               1563604
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.703
_shelx_estimated_absorpt_t_max   0.877
_shelx_res_checksum              440
_shelx_hkl_checksum              21900