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_1549631
_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         'C47 H81 B Fe N3 P3 Si2'
_chemical_formula_sum            'C47 H81 B Fe N3 P3 Si2'
_chemical_formula_weight         903.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-28
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3085(5)
_cell_length_b                   24.2407(12)
_cell_length_c                   37.5101(18)
_cell_measurement_reflns_used    9023
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.41
_cell_measurement_theta_min      2.52
_cell_volume                     10282.5(8)
_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      99.97
_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  0.0714
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            222575
_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         32.032
_diffrn_reflns_theta_min         2.522
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1040 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.8682. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         17889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.002
_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^+15.7260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15107
_reflns_number_total             17889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02380h2.cif
_cod_data_source_block           Complex9
_cod_depositor_comments
'Adding full bibliography for 1549629--1549633.cif.'
_cod_database_code               1549631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.880
_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
2.a Ternary CH refined with riding coordinates:
 C15(H15), C12(H12), C36(H36), C27(H27), C24(H24), C39(H39), B1(H1A)
2.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C19(H19), C34(H34), C22(H22), C7(H7), C21(H21), C20(H20),
 C8(H8), C33(H33), C31(H31), C32(H32)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C), C5(H5A,H5B,
 H5C), C4(H4A,H4B,H4C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C), C46(H46A,H46B,
 H46C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C37(H37A,
 H37B,H37C), C43(H43A,H43B,H43C), C28(H28A,H28B,H28C), C47(H47A,H47B,H47C),
 C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              91049
_olex2_submission_special_instructions 'No special instructions were received'