Stereogenic-at-iron mesoionic carbene complex for enantioselective C-H amidation.
Demirel, Nemrud; Dawor, Mahiob; Nadler, Greta; Ivlev, Sergei I.; Meggers, Eric; Chemical science 15 (2024) 15625–15631; doi:10.1039/d4sc03504f

data_1572557
_publ_section_title
;
 Stereogenic-at-iron mesoionic carbene complex for enantioselective C-H
 amidation.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              15625
_journal_page_last               15631
_journal_paper_doi               10.1039/d4sc03504f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C40 H40 F6 Fe N10, 2(F6 P)'
_chemical_formula_sum            'C40 H40 F18 Fe N10 P2'
_chemical_formula_weight         1120.61
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-04-08 deposited with the CCDC.	2024-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.5190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6131(5)
_cell_length_b                   23.9374(9)
_cell_length_c                   16.1455(7)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.3004
_cell_measurement_theta_min      2.4147
_cell_volume                     4594.6(3)
_computing_cell_refinement       'APEX3 v2019.11-0 (Bruker AXS, 2019)'
_computing_data_collection       'APEX3 v2019.11-0 (Bruker AXS, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2019)'
_computing_molecular_graphics    'Diamond v4.6.6 (Brandenburg, 2021)'
_computing_publication_material  'XCIF v2014/2 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'PHOTON III C14'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.8 mm diameter'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            104762
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         2.165
_diffrn_source                   'microfocus X-ray tube'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_correction_T_min  0.8363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.141
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+4.1846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9444
_reflns_number_total             11416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc03504f2.cif
_cod_data_source_block           iND049
_cod_depositor_comments
'Adding full bibliography for 1572557--1572559.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1572557
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_checksum              58316
_shelx_hkl_checksum              57865