Electrophile-promoted Fe-to-N<sub>2</sub> hydride migration in highly reduced Fe(N<sub>2</sub>)(H) complexes.
Deegan, Meaghan M.; Peters, Jonas C.; Chemical science 9 (2018) 6264–6270; doi:10.1039/c8sc02380h

data_1549630
_publ_section_title
;
 Electrophile-promoted Fe-to-N<sub>2</sub> hydride migration in highly
 reduced Fe(N<sub>2</sub>)(H) complexes.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              6264
_journal_page_last               6270
_journal_paper_doi               10.1039/c8sc02380h
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C36 H55 B Fe N2 P3, C28 H40 K O10'
_chemical_formula_sum            'C64 H95 B Fe K N2 O10 P3'
_chemical_formula_weight         1251.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-30 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.8390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3464(4)
_cell_length_b                   35.5398(14)
_cell_length_c                   15.8541(6)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.27
_cell_measurement_theta_min      2.47
_cell_volume                     6392.5(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0808
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            181071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.142
_diffrn_reflns_theta_min         2.130
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0615 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.9419. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     986
_refine_ls_number_reflns         24375
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0330P)^2^+2.3710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19008
_reflns_number_total             24375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02380h2.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
'Adding full bibliography for 1549629--1549633.cif.'
_cod_database_code               1549630
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C33B, C33A, C31B, C31A, C32B, C32A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23B, C23A, C22B, C22A, C24A, C24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O10B, O9B, O6B, O7A, O8A, C61A, C62A, C60A, C63A, C51A, C64A, C56A, C59A,
 C58A, C57A, C52A, C55A, C54A, C53A, C56B, C51B, C52B, C53B, C54B, C55B, O7B,
 C57B, C58B, O8B, C58B, C60B, C62B, C63B, C64B, O6A, O10A, C61B, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O10B)=Sof(O9B)=Sof(O6B)=Sof(C56B)=Sof(C51B)=Sof(C52B)=Sof(H52B)=Sof(C53B)=
 Sof(H53B)=Sof(C54B)=Sof(H54B)=Sof(C55B)=Sof(H55B)=Sof(O7B)=Sof(C57B)=Sof(H57C)=
 Sof(H57D)=Sof(C58B)=Sof(H58C)=Sof(H58D)=Sof(O8B)=Sof(C59B)=Sof(H59C)=Sof(H59D)=
 Sof(C60B)=Sof(H60C)=Sof(H60D)=Sof(C62B)=Sof(H62C)=Sof(H62D)=Sof(C63B)=
 Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64C)=Sof(H64D)=Sof(C61B)=Sof(H61C)=
 Sof(H61D)=1-FVAR(1)
 Sof(O7A)=Sof(O8A)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=Sof(H62B)=
 Sof(C60A)=Sof(H60A)=Sof(H60B)=Sof(C63A)=Sof(H63A)=Sof(H63B)=Sof(C51A)=
 Sof(C64A)=Sof(H64A)=Sof(H64B)=Sof(C56A)=Sof(C59A)=Sof(H59A)=Sof(H59B)=
 Sof(C58A)=Sof(H58A)=Sof(H58B)=Sof(C57A)=Sof(H57A)=Sof(H57B)=Sof(C52A)=
 Sof(H52A)=Sof(C55A)=Sof(H55A)=Sof(C54A)=Sof(H54A)=Sof(C53A)=Sof(H53A)=Sof(O6A)=
 Sof(O10A)=Sof(O9A)=FVAR(1)
 Sof(C22B)=Sof(H22B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23B)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C32A)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C22A)=Sof(H22A)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C19(H19), C34(H34), C10(H10), C7(H7), C31A(H31A), C22A(H22A), C22B(H22B),
 C31B(H31B)
4.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C43(H43A,H43B), C61A(H61A,H61B), C62A(H62A,H62B), C38(H38A,
 H38B), C60A(H60A,H60B), C63A(H63A,H63B), C42(H42A,H42B), C64A(H64A,H64B),
 C37(H37A,H37B), C41(H41A,H41B), C59A(H59A,H59B), C58A(H58A,H58B), C40(H40A,
 H40B), C39(H39A,H39B), C57A(H57A,H57B), C57B(H57C,H57D), C58B(H58C,H58D),
 C59B(H59C,H59D), C60B(H60C,H60D), C62B(H62C,H62D), C63B(H63C,H63D), C64B(H64C,
 H64D), C61B(H61C,H61D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C27(H27), C28(H28), C26(H26), C15(H15), C4(H4), C5(H5), C16(H16),
 C14(H14), C29(H29), C17(H17), C3(H3), C46(H46), C47(H47), C49(H49), C48(H48),
 C52A(H52A), C55A(H55A), C54A(H54A), C53A(H53A), C52B(H52B), C53B(H53B),
 C54B(H54B), C55B(H55B)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C11(H11A,H11B,H11C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C23A(H23A,H23B,
 H23C), C21(H21A,H21B,H21C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C),
 C24A(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C23B(H23D,H23E,H23F), C33B(H33D,
 H33E,H33F), C32B(H32D,H32E,H32F)
;
_shelx_res_checksum              89022
_olex2_submission_special_instructions 'No special instructions were received'