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_1559855
_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         'C45 H50 B2 Fe N10 O'
_chemical_formula_sum            'C45 H50 B2 Fe N10 O'
_chemical_formula_weight         824.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-19
_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                 98.957(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7182(7)
_cell_length_b                   24.1607(11)
_cell_length_c                   23.6620(9)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.204
_cell_measurement_theta_min      2.389
_cell_volume                     10570.5(7)
_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 0.985
_diffrn_measured_fraction_theta_max 0.984
_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  0.0704
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19096
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.348
_diffrn_reflns_theta_min         1.828
_exptl_absorpt_coefficient_mu    2.588
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0798 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.7379. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_description       block
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.145
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         19096
_refine_ls_number_restraints     542
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0677
_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^)+(0.1188P)^2^+1.7449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13918
_reflns_number_total             19096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06466a2.cif
_cod_data_source_block           ln620_nh_sq
_cod_depositor_comments
;Adding full bibliography for 1559850--1559855.cif.

 Adding full bibliography for 1559850--1559855.cif.
;
_cod_database_code               1559855
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.656
_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
 C66A-C70A \\sim C70A-C68A \\sim C66-C70 \\sim C68-C70
 with sigma of 0.02
 C11-C13 \\sim C9-C13 \\sim C13A-C11A \\sim C9A-C13A
 with sigma of 0.02
 C7-B1 \\sim C7A-B1
 with sigma of 0.02
 C13A-C10A \\sim C13-C10
 with sigma of 0.01
 C64-B4 \\sim C64A-B4
 with sigma of 0.02
 C70A-C67A \\sim C70-C67
 with sigma of 0.01
 Fe1-H10 \\sim H20-Fe2
 with sigma of 0.02
 C90A-C81 \\sim C90-C81 \\sim C88A-C81 \\sim C88-C81 \\sim C89A-C81 \\sim
C89-C81
 with sigma of 0.02
 C89A-C90A \\sim C89-C90 \\sim C90A-C88A \\sim C90-C88 \\sim C88A-C89A \\sim
C88-C89
 with sigma of 0.02
 C90A-C87 \\sim C90-C87 \\sim C88A-C87 \\sim C88-C87 \\sim C89A-C87 \\sim
C89-C87
 with sigma of 0.01
3. Restrained planarity
 C10, C11, C12, C7, C8, C9, C13
 with sigma of 0.1
 C13A, C11A, C12A, C8A, C7A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12 \\sim C7 \\sim C8 \\sim C9 \\sim C13 \\sim C11A \\sim
C12A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C13A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C64A
\\sim C65A \\sim C66A \\sim C67A \\sim C68A \\sim C69A \\sim C70A: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C89A) \\sim Ueq, Uanis(C88A) \\sim Ueq, Uanis(C90A) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=1-FVAR(1)
 Sof(C10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(C9)=
 Sof(H9)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=FVAR(1)
 Sof(C64A)=Sof(C69A)=Sof(H69A)=Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(C66A)=
 Sof(H66A)=Sof(C65A)=Sof(H65A)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=1-FVAR(2)
 Sof(C64)=Sof(C69)=Sof(H69)=Sof(C68)=Sof(H68)=Sof(C67)=Sof(C66)=Sof(H66)=
 Sof(C65)=Sof(H65)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=FVAR(2)
 Sof(C89A)=Sof(H89D)=Sof(H89E)=Sof(H89F)=Sof(C88A)=Sof(H88D)=Sof(H88E)=
 Sof(H88F)=Sof(C90A)=Sof(H90D)=Sof(H90E)=Sof(H90F)=1-FVAR(3)
 Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=Sof(C89)=Sof(H89A)=Sof(H89B)=Sof(H89C)=
 Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(H90C)=FVAR(3)
6.a Me refined with riding coordinates:
 C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C89A(H89D,H89E,
 H89F), C88A(H88D,H88E,H88F), C90A(H90D,H90E,H90F)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C8(H8),
 C9(H9), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20A), C21(H21), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C35(H35), C37(H37),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C53(H53),
 C54(H54), C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C69(H69), C68(H68),
  C66(H66), C65(H65), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
 C76(H76), C80(H80), C82(H82), C11A(H11A), C12A(H12A), C8A(H8A), C9A(H9A),
 C69A(H69A), C68A(H68A), C66A(H66A), C65A(H65A)
6.c Fitted hexagon refined as free rotating group:
 C10(C11,C12,C7,C8,C9), C64(C69,C68,C67,C66,C65), C11A(C12A,C7A,C8A,C9A,C10A),
 C64A(C69A,C68A,C67A,C66A,C65A)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C58(H58A,H58B,H58C), C70(H70A,H70B,H70C), C84(H84A,H84B,H84C),
 C85(H85A,H85B,H85C), C86(H86A,H86B,H86C), C13A(H13D,H13E,H13F), C70A(H70D,H70E,
 H70F)
;
_shelx_res_checksum              78959
_shelx_fab_checksum              75435
_olex2_submission_special_instructions 'No special instructions were received'