Mechanism of the Selective Fe-Catalyzed Arene Carbon‒Hydrogen Bond Functionalization
Postils, Verònica; Rodríguez, Mònica; Sabenya, Gerard; Conde, Ana; Díaz-Requejo, M. Mar; Pérez, Pedro J.; Costas, Miquel; Solà, Miquel; Luis, Josep M.; ACS Catalysis 8 (2018) 4313–; doi:10.1021/acscatal.7b03935

data_4515624
_publ_section_title
;
 Mechanism of the Selective Fe-Catalyzed Arene Carbon--Hydrogen Bond
 Functionalization
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4313
_journal_paper_doi               10.1021/acscatal.7b03935
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety
'C32 H12 B F24, 0.5(C30 H48 F6 Fe2 N8 O6 S2), C H2 Cl2'
_chemical_formula_sum            'C48 H38 B Cl2 F27 Fe N4 O3 S'
_chemical_formula_weight         1401.44
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                102.363(2)
_cell_angle_beta                 97.011(2)
_cell_angle_gamma                92.487(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6950(11)
_cell_length_b                   13.3351(11)
_cell_length_c                   17.1823(15)
_cell_measurement_reflns_used    8004
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.17
_cell_volume                     2812.8(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43857
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.285
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.765601
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         13585
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1055
_refine_ls_R_factor_gt           0.0726
_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^)+(0.0789P)^2^+2.3557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1656
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9340
_reflns_number_total             13585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03935_si_003.cif
_cod_data_source_block           mrc181_1_sq_s
_cod_database_code               4515624
_shelxl_version_number           2013-3
_shelx_res_checksum              25769
_shelx_hkl_checksum              12703
_shelx_fab_checksum              89981