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_1543381
_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 H41 B2 Fe N10, 2(C3 H3)'
_chemical_formula_sum            'C45 H47 B2 Fe N10'
_chemical_formula_weight         805.39
_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-2013
_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                   16.6523(3)
_cell_length_b                   10.1363(2)
_cell_length_c                   29.6556(6)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.35
_cell_measurement_theta_min      2.98
_cell_volume                     5005.65(17)
_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.  5.3.0'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            31260
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.577
_diffrn_reflns_theta_min         2.980
_exptl_absorpt_coefficient_mu    2.708
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.408
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5223
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0746P)^2^+2.2167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4800
_reflns_number_total             5223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc01433j2.cif
_cod_data_source_block           2Ad
_cod_depositor_comments
'Adding full bibliography for 1543379--1543384.cif.'
_cod_database_code               1543381
_shelxl_version_number           2013-4
_shelx_res_checksum              35056