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_1549632
_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         'C49 H85 B Fe K N2 O P3 Si'
_chemical_formula_sum            'C49 H85 B Fe K N2 O P3 Si'
_chemical_formula_weight         944.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-30 deposited with the CCDC.
2018-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                97.411(10)
_cell_angle_beta                 95.734(4)
_cell_angle_gamma                117.826(8)
_cell_formula_units_Z            2
_cell_length_a                   12.4653(18)
_cell_length_b                   13.091(3)
_cell_length_c                   21.997(3)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.91
_cell_measurement_theta_min      2.66
_cell_volume                     3095.0(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-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0522
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            173434
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.044
_diffrn_reflns_theta_min         2.255
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.7201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0758 before and 0.0521 after correction. The Ratio of minimum to maximum transmission is 0.9644. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.014
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         25264
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0500P)^2^+0.9140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1014
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20001
_reflns_number_total             25264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02380h2.cif
_cod_data_source_block           Complex5
_cod_depositor_comments
'Adding full bibliography for 1549629--1549633.cif.'
_cod_original_cell_volume        3095.1(10)
_cod_database_code               1549632
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.889
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Rigid body (RIGU) restrains
 C46A, C47A, C48A, C49A, O1, O2, C49B, C48B, C47B, C46B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C43B)=Sof(H43B)=Sof(C44B)=Sof(H44D)=
 Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=
 Sof(H44B)=Sof(H44C)=FVAR(1)
 Sof(O2)=Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C47B)=
 Sof(H47C)=Sof(H47D)=Sof(C46B)=Sof(H46C)=Sof(H46D)=1-FVAR(2)
 Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(C48A)=
 Sof(H48A)=Sof(H48B)=Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(O1)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C22(H22), C31(H31), C37(H37), C7(H7), C10(H10), C43A(H43A), B1(H1), C34(H34),
 C40(H40), C19(H19), C43B(H43B)
4.b Secondary CH2 refined with riding coordinates:
 C46A(H46A,H46B), C47A(H47A,H47B), C48A(H48A,H48B), C49A(H49A,H49B), C49B(H49C,
 H49D), C48B(H48C,H48D), C47B(H47C,H47D), C46B(H46C,H46D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C29(H29), C28(H28), C15(H15), C26(H26), C27(H27), C5(H5), C18(H18),
 C16(H16), C4(H4), C17(H17), C6(H6)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C45(H45A,H45B,
 H45C), C45(H45D,H45E,H45F), C39(H39A,H39B,H39C), C35(H35A,H35B,H35C), C8(H8A,
 H8B,H8C), C11(H11A,H11B,H11C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C),
 C33(H33A,H33B,H33C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C41(H41A,H41B,H41C), C44A(H44A,H44B,H44C),
 C12(H12A,H12B,H12C), C44B(H44D,H44E,H44F)
;
_shelx_res_checksum              88003
_shelx_fab_checksum              21489
_olex2_submission_special_instructions 'No special instructions were received'