Spin polarization assisted facile C-H activation by an <i>S</i> = 1 iron(iv)-bisimido complex: a comprehensive spectroscopic and theoretical investigation.
Xiong, Jin; Liu, Qing; Lavina, Barbara; Hu, Michael Y.; Zhao, Jiyong; Alp, Esen E.; Deng, Liang; Ye, Shengfa; Guo, Yisong; Chemical science 14 (2023) 2808–2820; doi:10.1039/d2sc06273a

data_1568418
_publ_section_title
;
 Spin polarization assisted facile C-H activation by an <i>S</i> = 1
 iron(iv)-bisimido complex: a comprehensive spectroscopic and theoretical
 investigation.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              2808
_journal_page_last               2820
_journal_paper_doi               10.1039/d2sc06273a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C51 H70 Fe N4'
_chemical_formula_sum            'C51 H70 Fe N4'
_chemical_formula_weight         794.96
_chemical_properties_physical    Air-sensitive,Hygroscopic,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-13 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.448(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.1585(7)
_cell_length_b                   9.2604(3)
_cell_length_c                   23.5718(7)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.97
_cell_measurement_theta_min      3.33
_cell_volume                     4601.9(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20345
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.942
_diffrn_reflns_theta_min         4.537
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0973 before and 0.0571 after correction. The Ratio of minimum to maximum transmission is 0.8275. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether and THF'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0557P)^2^+5.1281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3874
_reflns_number_total             4317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06273a2.cif
_cod_data_source_block           mj19383_0m
_cod_depositor_comments          'Adding full bibliography for 1568418.cif.'
_cod_database_code               1568418
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13B,H13A,H13C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              31054
_olex2_submission_special_instructions 'No special instructions were received'