High-Spin Iron Imido Complexes Competent for C-H Bond Amination.
Wilding, Matthew J. T.; Iovan, Diana A.; Betley, Theodore A.; Journal of the American Chemical Society 139 (2017) 12043–12049; doi:10.1021/jacs.7b06682

data_4131543
_publ_section_title
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 High-Spin Iron Imido Complexes Competent for C-H Bond Amination.
;
_journal_issue                   34
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12043
_journal_page_last               12049
_journal_paper_doi               10.1021/jacs.7b06682
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C66 H48.92 Fe N2, 3(C6 H6)'
_chemical_formula_sum            'C84 H66.92 Fe N2'
_chemical_formula_weight         1160.16
_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
_audit_creation_date             2014-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                76.0078(10)
_cell_angle_beta                 83.8575(11)
_cell_angle_gamma                64.8883(9)
_cell_formula_units_Z            2
_cell_length_a                   12.5156(2)
_cell_length_b                   13.9784(2)
_cell_length_c                   20.1391(3)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      70.159
_cell_measurement_theta_min      2.261
_cell_volume                     3095.58(9)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.3.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XLMP (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type
;
Bruker D8 goniometer with CCD area detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77844
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.161
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'I\mS microfocus tube'
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.7736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       plate
_exptl_crystal_F_000             1222
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         11081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0626P)^2^+1.8320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8892
_reflns_number_total             11081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06682_si_002.cif
_cod_data_source_block           mw2
_cod_original_cell_volume        3095.59(8)
_cod_database_code               4131543
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.629
_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
Uanis(C2) = Uanis(C2A)
Uanis(C2AA) = Uanis(C2AB)
Uanis(C1) = Uanis(C1A)
Uanis(C3AA) = Uanis(C3AB)
Uanis(C4AA) = Uanis(C4AB)
Uanis(C5AA) = Uanis(C5AB)
Uanis(Fe1) = Uanis(Fe1A)
Uanis(N2) = Uanis(N2A)
Uanis(N1) = Uanis(N1A)
Uanis(C8) = Uanis(C8A)
Uanis(C26) = Uanis(C26A)
3. Others
 Sof(H11A)=Sof(H30)=Sof(H44A)=Sof(Fe1A)=Sof(N2A)=Sof(N1A)=Sof(C8A)=Sof(C26A)=1-
 FVAR(1)
 Sof(Fe1)=Sof(N1)=Sof(N2)=Sof(C8)=Sof(H11)=Sof(C26)=Sof(H43)=Sof(H44)=Sof(H55)=
 FVAR(1)
 Sof(C2A)=Sof(H2A)=Sof(C2AB)=Sof(H2AB)=Sof(C1A)=Sof(H1A)=Sof(C3AB)=Sof(H3AB)=
 Sof(C4AB)=Sof(H4AB)=Sof(C5AB)=Sof(H5AB)=1-FVAR(2)
 Sof(C2)=Sof(H2)=Sof(C5AA)=Sof(H5AA)=Sof(C4AA)=Sof(H4AA)=Sof(C3AA)=Sof(H3AA)=
 Sof(C1)=Sof(H1)=Sof(C2AA)=Sof(H2AA)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C30(H30)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C11(H11A), C12(H12), C15(H15), C18(H18), C19(H19), C21(H21),
 C23(H23), C24(H24), C27(H27), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37),
  C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C44(H44A), C45(H45),
 C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54),
  C55(H55), C57(H57), C58(H58), C59(H59), C61(H61), C63(H63), C64(H64),
 C68(H68), C71(H71), C73(H73), C74(H74), C77(H77), C60(H60), C62(H62), C65(H65),
  C67(H67), C70(H70), C78(H78), C72(H72), C75(H75), C76(H76), C81(H81),
 C0AA(H0AA), C1AA(H1AA), C2(H2), C5AA(H5AA), C4AA(H4AA), C3AA(H3AA), C1(H1),
 C2AA(H2AA), C2A(H2A), C2AB(H2AB), C1A(H1A), C3AB(H3AB), C4AB(H4AB), C5AB(H5AB)
4.c Fitted hexagon refined as free rotating group:
 C2(C5AA,C4AA,C3AA,C1,C2AA), C2A(C2AB,C1A,C3AB,C4AB,C5AB)
4.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C56(H56A,H56B,H56C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              35752
_shelx_hkl_checksum              34068