Activation of ammonia and hydrazine by electron rich Fe(ii) complexes supported by a dianionic pentadentate ligand platform through a common terminal Fe(iii) amido intermediate.
Nurdin, Lucie; Yang, Yan; Neate, Peter G. N.; Piers, Warren E.; Maron, Laurent; Neidig, Michael L.; Lin, Jian-Bin; Gelfand, Benjamin S.; Chemical science 12 (2020) 2231–2241; doi:10.1039/d0sc06466a

data_1559852
_publ_section_title
;
 Activation of ammonia and hydrazine by electron rich Fe(ii) complexes
 supported by a dianionic pentadentate ligand platform through a common
 terminal Fe(iii) amido intermediate.
;
_journal_issue                   6
_journal_name_full               'Chemical science'
_journal_page_first              2231
_journal_page_last               2241
_journal_paper_doi               10.1039/d0sc06466a
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'F6 Sb, C31 H32 B2 Fe N10, C6 H6'
_chemical_formula_sum            'C37 H38 B2 F6 Fe N10 Sb'
_chemical_formula_weight         935.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-14 deposited with the CCDC.	2020-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.2040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9800(2)
_cell_length_b                   25.1657(5)
_cell_length_c                   14.4893(3)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.811
_cell_measurement_theta_min      3.777
_cell_volume                     3984.30(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            28060
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.065
_diffrn_reflns_theta_min         3.512
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.900
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.6567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0512 before and 0.0406 after correction. The Ratio of minimum to maximum transmission is 0.8715. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.416
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0617P)^2^+4.0072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6088
_reflns_number_total             7559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06466a2.cif
_cod_data_source_block           ln582red
_cod_depositor_comments
;Adding full bibliography for 1559850--1559855.cif.

 Adding full bibliography for 1559850--1559855.cif.
;
_cod_original_cell_volume        3984.29(14)
_cod_database_code               1559852
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.559
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24),
  C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C1S(H1S),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S)
2.b Idealised Me refined as rotating group:
 N10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              71805
_olex2_submission_special_instructions 'No special instructions were received'