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_1559850
_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 H32 B2 Fe N10, C6 H6'
_chemical_formula_sum            'C37 H38 B2 Fe N10'
_chemical_formula_weight         700.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-04
_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                 102.636(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6461(14)
_cell_length_b                   17.2299(16)
_cell_length_c                   24.132(2)
_cell_measurement_reflns_used    8710
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.226
_cell_measurement_theta_min      3.740
_cell_volume                     6753.7(10)
_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
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_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  0.0545
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            18406
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.291
_diffrn_reflns_theta_min         3.740
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.928
_exptl_absorpt_correction_T_max  0.6554
_exptl_absorpt_correction_T_min  0.4822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0908 before and 0.0370 after correction. The Ratio of minimum to maximum transmission is 0.7357. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6138
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0818P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4514
_reflns_number_total             6138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06466a2.cif
_cod_data_source_block           ln585
_cod_depositor_comments
;Adding full bibliography for 1559850--1559855.cif.

 Adding full bibliography for 1559850--1559855.cif.
;
_cod_database_code               1559850
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.405
_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. Restrained distances
 N10-H10A = N10-H10B = N10-H10C
 0.91 with sigma of 0.02
 H10A-H10C
 1.49 with sigma of 0.04
 H10C-H10B
 1.49 with sigma of 0.04
 H10B-H10A
 1.49 with sigma of 0.04
 C1S-C2S \\sim C1T-C2T
 with sigma of 0.02
 C1S-C6S \\sim C1T-C6T
 with sigma of 0.02
 C2S-C3S \\sim C2T-C3T
 with sigma of 0.02
 C3S-C4S \\sim C3T-C4T
 with sigma of 0.02
 C4S-C5S \\sim C4T-C5T
 with sigma of 0.02
 C5S-C6S \\sim C5T-C6T
 with sigma of 0.02
 C1S-C3S \\sim C1T-C3T
 with sigma of 0.04
 C1S-C5S \\sim C1T-C5T
 with sigma of 0.04
 C2S-C4S \\sim C2T-C4T
 with sigma of 0.04
 C2S-C6S \\sim C2T-C6T
 with sigma of 0.04
 C3S-C5S \\sim C3T-C5T
 with sigma of 0.04
 C4S-C6S \\sim C4T-C6T
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C6S \\sim C1S \\sim C2S \\sim C3S \\sim C5S \\sim C4S: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C1T \\sim C6T \\sim C2T \\sim C5T \\sim C3T \\sim C4T: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C1T, C6T, C2T, C5T, C3T, C4T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6S, C1S, C2S, C3S, C5S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6T)=Sof(H6T)=Sof(C1T)=Sof(H1T)=Sof(C2T)=Sof(H2T)=Sof(C3T)=Sof(H3T)=
 Sof(C4T)=Sof(H4T)=Sof(C5T)=Sof(H5T)=1-FVAR(1)
 Sof(C1S)=Sof(H1S)=Sof(C2S)=Sof(H2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=
 Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=FVAR(1)
6.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), 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), C6T(H6T), C1T(H1T), C2T(H2T),
  C3T(H3T), C4T(H4T), C5T(H5T)
6.b Fitted hexagon refined as free rotating group:
 C1S(C2S,C3S,C4S,C5S,C6S), C6T(C1T,C2T,C3T,C4T,C5T)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              67301
_olex2_submission_special_instructions 'No special instructions were received'