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_4129690
_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         'C45 H58 Fe N4'
_chemical_formula_sum            'C45 H58 Fe N4'
_chemical_formula_weight         710.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                67.416(6)
_cell_angle_beta                 73.222(6)
_cell_angle_gamma                66.689(5)
_cell_formula_units_Z            2
_cell_length_a                   11.046(4)
_cell_length_b                   13.437(5)
_cell_length_c                   15.899(6)
_cell_measurement_reflns_used    1951
_cell_measurement_temperature    130
_cell_measurement_theta_max      21.61
_cell_measurement_theta_min      2.28
_cell_volume                     1974.8(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0654
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14579
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.734
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0796 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.6308.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0869
_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^)+(0.1243P)^2^+2.2471P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2309
_refine_ls_wR_factor_ref         0.2674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4495
_reflns_number_total             7751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09579_si_002.cif
_cod_data_source_block           7
_cod_original_cell_volume        1974.9(12)
_cod_database_code               4129690
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C30(H30), C33(H33), C43(H43)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C17(H17), C19(H19),
 C26(H26), C27(H27), C28(H28), C38(H38), C39(H39), C40(H40)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C42(H42A,H42B,H42C),
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              49512
_shelx_hkl_checksum              61402
_olex2_submission_special_instructions 'No special instructions were received'