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_1559851
_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         'C62 H60 B4 Fe2 N20, C3 H3'
_chemical_formula_sum            'C65 H63 B4 Fe2 N20'
_chemical_formula_weight         1279.29
_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     dual
_audit_creation_date             2019-08-23
_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                98.128(5)
_cell_angle_beta                 100.359(5)
_cell_angle_gamma                115.218(5)
_cell_formula_units_Z            2
_cell_length_a                   12.5636(9)
_cell_length_b                   13.6840(10)
_cell_length_c                   20.5835(17)
_cell_measurement_reflns_used    3745
_cell_measurement_temperature    173
_cell_measurement_theta_max      69.99
_cell_measurement_theta_min      3.68
_cell_volume                     3053.3(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.973
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10913
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.355
_diffrn_reflns_theta_min         2.251
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.291
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1073 before and 0.0372 after correction. The Ratio of minimum to maximum transmission is 0.8156. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       plank
_exptl_crystal_F_000             1330
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.485
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         10913
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0815P)^2^+0.1435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7603
_reflns_number_total             10913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06466a2.cif
_cod_data_source_block           ln634
_cod_depositor_comments
;Adding full bibliography for 1559850--1559855.cif.

 Adding full bibliography for 1559850--1559855.cif.
;
_cod_database_code               1559851
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.413
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 N10-H10 \\sim N11-H11
 with sigma of 0.02
 H10-N11 \\sim N10-H11
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C53(H53), C35(H35), C19(H19), C17(H17), C3(H3), C15(H15), C46(H46), C20(H20),
 C1(H1), C48(H48), C26(H26), C4(H4), C50(H50), C32(H32), C55(H55), C54(H54),
 C52(H52), C22(H22), C24(H24), C21(H21), C58(H58), C8(H8), C5(H5), C57(H57),
 C43(H43), C47(H47), C16(H16), C37(H37), C6(H6), C30(H30), C33(H33), C42(H42),
 C34(H34), C61(H61), C51(H51), C23(H23), C2(H2), C27(H27), C36(H36), C60(H60),
 C39(H39), C29(H29), C9(H9), C12(H12), C40(H40), C11(H11A), C1S(H1S), C3S(H3S),
 C2S(H2S)
3.b Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C62(H62A,H62B,H62C), C13(H13A,H13B,H13C), C31(H31A,H31B,
 H31C)
;
_shelx_res_checksum              4357
_olex2_submission_special_instructions 'No special instructions were received'