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_4129688
_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 H61 Fe N3'
_chemical_formula_sum            'C40 H61 Fe N3'
_chemical_formula_weight         639.76
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.4930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9259(9)
_cell_length_b                   25.8507(14)
_cell_length_c                   18.8349(10)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    130
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.35
_cell_volume                     7111.5(7)
_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 0.996
_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  0.0641
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.608
_diffrn_reflns_theta_min         1.418
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.455
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0623 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.8669.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         21814
_refine_ls_number_restraints     636
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+3.9437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13775
_reflns_number_total             21814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09579_si_002.cif
_cod_data_source_block           5
_cod_database_code               4129688
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.876
_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. Shared sites
{C77, C77'}
3. Uiso/Uaniso restraints and constraints
C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40 \\sim C41 \\sim C32' \\sim C33' \\sim C34' \\sim C35' \\sim C36' \\sim C37'
\\sim C38' \\sim C39' \\sim C40' \\sim C41': within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C71 \\sim C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim
C79 \\sim C80 \\sim C71' \\sim C72' \\sim C73' \\sim C74' \\sim C75' \\sim C76'
\\sim C77' \\sim C78' \\sim C79' \\sim C80': within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C77) = Uanis(C77')
4. Others
 Sof(C32')=Sof(C33')=Sof(H33C)=Sof(H33D)=Sof(C34')=Sof(H34A)=Sof(H34B)=
 Sof(C35')=Sof(H35')=Sof(C36')=Sof(H36A)=Sof(H36B)=Sof(C37')=Sof(H37C)=
 Sof(H37D)=Sof(C38')=Sof(H38')=Sof(C39')=Sof(H39A)=Sof(H39B)=Sof(C40')=
 Sof(H40')=Sof(C41')=Sof(H41C)=Sof(H41D)=1-FVAR(1)
 Sof(C32)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=
 Sof(H38B)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=
 Sof(H41B)=FVAR(1)
 Fixed Sof: C71(0.5) C72(0.5) H72A(0.5) H72B(0.5) C73(0.5) H73(0.5) C74(0.5)
 H74A(0.5) H74B(0.5) C75(0.5) H75(0.5) C76(0.5) H76A(0.5) H76B(0.5) C77(0.5)
 H77A(0.5) H77B(0.5) C78(0.5) H78(0.5) C79(0.5) H79A(0.5) H79B(0.5) C80(0.5)
 H80A(0.5) H80B(0.5) C71'(0.5) C72'(0.5) H72C(0.5) H72D(0.5) C73'(0.5)
 H73A(0.5) H73B(0.5) C74'(0.5) H74'(0.5) C75'(0.5) H75A(0.5) H75B(0.5)
 C76'(0.5) H76C(0.5) H76D(0.5) C77'(0.5) H77'(0.5) C78'(0.5) H78A(0.5)
 H78B(0.5) C79'(0.5) H79'(0.5) C80'(0.5) H80C(0.5) H80D(0.5)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C24(H24), C26(H26), C29(H29), C34(H34), C36(H36),
 C39(H39), C35'(H35'), C38'(H38'), C40'(H40'), C55(H55), C58(H58), C63(H63),
 C65(H65), C68(H68), C73(H73), C75(H75), C78(H78), C74'(H74'), C77'(H77'),
 C79'(H79')
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B), C28(H28A,H28B),
 C30(H30A,H30B), C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B),
  C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B), C33'(H33C,H33D), C34'(H34A,
 H34B), C36'(H36A,H36B), C37'(H37C,H37D), C39'(H39A,H39B), C41'(H41C,H41D),
 C43(H43A,H43B), C62(H62A,H62B), C64(H64A,H64B), C66(H66A,H66B), C67(H67A,H67B),
  C69(H69A,H69B), C70(H70A,H70B), C72(H72A,H72B), C74(H74A,H74B), C76(H76A,
 H76B), C77(H77A,H77B), C79(H79A,H79B), C80(H80A,H80B), C72'(H72C,H72D),
 C73'(H73A,H73B), C75'(H75A,H75B), C76'(H76C,H76D), C78'(H78A,H78B), C80'(H80C,
 H80D)
5.c Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C)
5.d Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C51(H51), C52(H52), C53(H53)
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_shelx_res_checksum              96635
_shelx_hkl_checksum              38563
_olex2_submission_special_instructions 'No special instructions were received'