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_1559853
_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         'C31 H29 B2 Br Fe N9, 2(C6 H6)'
_chemical_formula_sum            'C43 H41 B2 Br Fe N9'
_chemical_formula_weight         841.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-20
_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                104.192(5)
_cell_angle_beta                 92.618(5)
_cell_angle_gamma                112.901(5)
_cell_formula_units_Z            2
_cell_length_a                   10.252(5)
_cell_length_b                   12.025(5)
_cell_length_c                   18.400(8)
_cell_measurement_reflns_used    1687
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.741
_cell_measurement_theta_min      2.304
_cell_volume                     2000.4(16)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.1247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26732
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.918
_exptl_absorpt_coefficient_mu    1.420
_exptl_absorpt_correction_T_max  0.9143
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0580 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.9242.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0189P)^2^+1.2216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4570
_reflns_number_total             7875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06466a2.cif
_cod_data_source_block           mo_ln512_0m_a
_cod_depositor_comments
;Adding full bibliography for 1559850--1559855.cif.

 Adding full bibliography for 1559850--1559855.cif.
;
_cod_original_cell_volume        2000.3(15)
_cod_database_code               1559853
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.848
_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 Riding coordinates:
 C31(H31a,H31b,H31c)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C1S(H1S),
 C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S),
  C10S(H10S), C11S(H11S), C12S(H12S)
2.c Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c)
;
_shelx_res_checksum              67552
_olex2_submission_special_instructions 'No special instructions were received'