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_1543382
_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         ' C39 H39 B2 Fe N10 '
_chemical_formula_sum            'C39 H39 B2 Fe N10'
_chemical_formula_weight         725.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-11-27 deposited with the CCDC.
2016-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.518(4)
_cell_length_b                   9.9742(14)
_cell_length_c                   13.8788(19)
_cell_measurement_reflns_used    4132
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.48
_cell_measurement_theta_min      3.19
_cell_volume                     3532.5(9)
_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.  5.3.7'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14679
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         67.483
_diffrn_reflns_theta_min         3.464
_exptl_absorpt_coefficient_mu    3.776
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1516
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3339
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0785P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2518
_reflns_number_total             3339
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01433j2.cif
_cod_data_source_block           2Ar
_cod_depositor_comments
'Adding full bibliography for 1543379--1543384.cif.'
_cod_original_cell_volume        3532.5(8)
_cod_database_code               1543382
_shelx_estimated_absorpt_t_min   0.704
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2014/6
_shelx_res_checksum              40689