Identification and Reactivity of Cyclometalated Iron(II) Intermediates in Triazole-Directed Iron-Catalyzed C-H Activation.
Boddie, Theresa E.; Carpenter, Stephanie H.; Baker, Tessa M.; DeMuth, Joshua C.; Cera, Gianpiero; Brennessel, William W.; Ackermann, Lutz; Neidig, Michael L.; Journal of the American Chemical Society 141 (2019) 12338–12345; doi:10.1021/jacs.9b05269

data_4128619
_publ_section_title
;
 Identification and Reactivity of Cyclometalated Iron(II) Intermediates in
 Triazole-Directed Iron-Catalyzed C-H Activation.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12338
_journal_page_last               12345
_journal_paper_doi               10.1021/jacs.9b05269
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C42 H34 Fe P2, 3(C6 H6)'
_chemical_formula_sum            'C60 H52 Fe P2'
_chemical_formula_weight         890.80
_chemical_name_common            neitw13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 103.062(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1339(18)
_cell_length_b                   10.2597(10)
_cell_length_c                   25.508(3)
_cell_measurement_reflns_used    4092
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      2.21
_cell_volume                     4622.9(8)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2017)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
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_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 0.993
_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  0.1204
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            71517
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.678
_diffrn_reflns_theta_min         1.639
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            'dark red'
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_exptl_crystal_description       block
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_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         13005
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0503P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7528
_reflns_number_total             13005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05269_si_004.cif
_cod_data_source_block           neitw13
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4128619
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.918
_shelx_res_checksum              92431
_shelx_hkl_checksum              33031