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_4131547
_publ_section_title
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 High-Spin Iron Imido Complexes Competent for C-H Bond Amination.
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_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         'C76 H65 Fe N3, C7 H8'
_chemical_formula_sum            'C83 H73 Fe N3'
_chemical_formula_weight         1168.29
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                85.219(4)
_cell_angle_beta                 68.727(4)
_cell_angle_gamma                66.885(4)
_cell_formula_units_Z            2
_cell_length_a                   13.519(3)
_cell_length_b                   16.325(3)
_cell_length_c                   16.530(3)
_cell_measurement_reflns_used    2843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.50
_cell_volume                     3119.2(11)
_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      99.97
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type
;
Bruker C8 goniometer with CCD area detector
;
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1918
_diffrn_reflns_av_unetI/netI     0.2990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23138
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         1.33
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0740 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8267.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         9905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.2304
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2381
_reflns_number_gt                3857
_reflns_number_total             9905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b06682_si_002.cif
_cod_data_source_block           mw1_a
_cod_original_cell_volume        3119.4(10)
_cod_database_code               4131547
_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. Uiso/Uaniso restraints and constraints
Uanis(C028) = Uanis(C029)
Uanis(C025) = Uanis(C02E)
Uanis(Fe01) = Uanis(C008)
Uanis(C00F) = Uanis(C00A)
3.a Ternary CH refined with riding coordinates:
 C028(H028), C02C(H02K), C02E(H02N)
3.b Secondary CH2 refined with riding coordinates:
 C025(H02A,H02B), C026(H02C,H02D), C027(H02E,H02F), C029(H02G,H02H), C02A(H02I,
 H02J), C02D(H02L,H02M)
3.c Aromatic/amide H refined with riding coordinates:
 C005(H005), C00B(H00B), C00D(H00D), C00F(H00F), C00I(H00I), C00K(H00K),
 C00L(H00L), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C00Z(H00Z), N010(H010), C011(H011), C013(H013), C014(H014),
 C015(H015), C017(H017), C019(H019), C01A(H01A), C01D(H01D), C01F(H01F),
 C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L),
 C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01Y(H01Z), C01Z(H01), C021(H021),
 C022(H022), C023(H023), C024(H024), C02B(H02O)
3.d Idealised Me refined as rotating group:
 C01V(H01B,H01C,H01E), C01W(H01V,H01W,H01X), C01X(H01Y,H,HA), C02F(H02P,H02Q,
 H02R)
;
_olex2_submission_special_instructions 'No special instructions were received'