Facile hydrogen atom transfer to iron(III) imido radical complexes supported by a dianionic pentadentate ligand
Spasyuk, Denis M.; Carpenter, Stephanie H.; Kefalidis, Christos E.; Piers, Warren E.; Neidig, Michael L.; Maron, Laurent; Chemical Science 7 (2016) 5939–5944; doi:10.1039/c6sc01433j

data_1543383
_publ_section_title
;
 Facile hydrogen atom transfer to iron(III) imido radical complexes
 supported by a dianionic pentadentate ligand
;
_journal_coden_ASTM              CSHCCN
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              5939
_journal_page_last               5944
_journal_paper_doi               10.1039/c6sc01433j
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C68 H63 B4 Fe2 N19 O2 S, C6 H6'
_chemical_formula_sum            'C74 H69 B4 Fe2 N19 O2 S'
_chemical_formula_weight         1443.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-11-27 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                68.407(3)
_cell_angle_beta                 83.226(3)
_cell_angle_gamma                68.207(3)
_cell_formula_units_Z            2
_cell_length_a                   13.5661(12)
_cell_length_b                   16.6230(14)
_cell_length_c                   19.6115(17)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.50
_cell_measurement_theta_min      2.42
_cell_volume                     3817.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'LinXTL v.  5.3.8'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54443
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.913
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    3.758
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.4073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         14328
_refine_ls_number_restraints     1386
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1228P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8717
_reflns_number_total             14328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01433j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1543379--1543384.cif.'
_cod_database_code               1543383
_shelx_estimated_absorpt_t_min   0.399
_shelx_estimated_absorpt_t_max   0.705
_shelxl_version_number           2013-4
_shelx_res_checksum              85961