Three-coordinate iron(IV) bisimido complexes with aminocarbene ligation: synthesis, structure, and reactivity.
Wang, Lei; Hu, Lianrui; Zhang, Hezhong; Chen, Hui; Deng, Liang; Journal of the American Chemical Society 137 (2015) 14196–14207; doi:10.1021/jacs.5b09579

data_4129689
_publ_section_title
;
 Three-coordinate iron(IV) bisimido complexes with aminocarbene ligation:
 synthesis, structure, and reactivity.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14196
_journal_page_last               14207
_journal_paper_doi               10.1021/jacs.5b09579
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C40 H57 Fe N3'
_chemical_formula_sum            'C40 H57 Fe N3'
_chemical_formula_weight         635.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8742(8)
_cell_length_b                   30.161(2)
_cell_length_c                   11.4324(8)
_cell_measurement_reflns_used    5938
_cell_measurement_temperature    130
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.26
_cell_volume                     3559.4(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35946
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.601
_diffrn_reflns_theta_min         1.994
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.454
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0527 before and 0.0457 after correction.
The Ratio of minimum to maximum transmission is 0.9211.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         10917
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0485P)^2^+1.1003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7845
_reflns_number_total             10917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09579_si_002.cif
_cod_data_source_block           6
_cod_original_cell_volume        3559.4(5)
_cod_database_code               4129689
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.857
_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. Uiso/Uaniso restraints and constraints
C4 \\sim C6 \\sim C3 \\sim C5: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C6' \\sim C5' \\sim C3': within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C4 \\sim C4' \\sim C5' \\sim C3' \\sim C3 \\sim C6 \\sim C5 \\sim C2 \\sim C6':
within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.08
Uanis(C4') \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 H5C(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5) C3'(0.5) H3'A(0.5) H3'B(0.5)
 C4'(0.5) C5'(0.5) H5'A(0.5) H5'B(0.5) H5'C(0.5) C6'(0.5) H6'A(0.5) H6'B(0.5)
 H6'C(0.5)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18)
4.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C3'(H3'A,H3'B), C24(H24A,H24B), C34(H34A,H34B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
4.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C5'(H5'A,H5'B,H5'C), C6'(H6'A,H6'B,H6'C),
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              74458
_shelx_hkl_checksum              82489
_olex2_submission_special_instructions 'No special instructions were received'