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_4131544
_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         'C86 H79 Fe N6'
_chemical_formula_sum            'C86 H79 Fe N6'
_chemical_formula_weight         1252.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                90
_cell_angle_beta                 98.769(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.529(8)
_cell_length_b                   18.634(8)
_cell_length_c                   47.04(2)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.88
_cell_measurement_theta_min      2.19
_cell_volume                     16052(12)
_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)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1267
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            122961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.970
_diffrn_reflns_theta_min         1.177
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.0955 before and 0.0773 after correction.
The Ratio of minimum to maximum transmission is 0.7734.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       plate
_exptl_crystal_F_000             5304
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.342
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         15588
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1586
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1921P)^2^+89.7327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3064
_refine_ls_wR_factor_ref         0.3463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10088
_reflns_number_total             15588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06682_si_002.cif
_cod_data_source_block           mono2_a
_cod_original_cell_volume        16051(12)
_cod_database_code               4131544
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.940
_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.a Ternary CH refined with riding coordinates:
 C00K(H00K), C01C(H01E), C01S(H01S), C01W(H01W), C026(H026), C029(H029)
2.b Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00D), C00P(H00E,H00F), C017(H01A,H01B), C01B(H01C,H01D), C01M(H01G,
 H01M), C01N(H01N,H01O), C01O(H01P,H01Q), C01U(H01T,H01U), C025(H02A,H02B),
 C027(H02C,H02D), C02A(H02E,H02F), C02E(H02I,H02J)
2.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00B(H00B), C00C(H00C), C00O(H00O), C00T(H00T), C00U(H00U),
 C00V(H00V), C00X(H00X), C00Z(H00Z), C013(H013), C015(H015), C016(H016),
 C018(H018), C019(H019), C01F(H01F), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01P(H01R), C01V(H01V), C01X(H01X), C01Z(H01Z),
 C020(H020), C021(H021), C022(H022), C023(H023), C028(H028), C02C(H02G),
 C02D(H02H), C02F(H02K), C02G(H02L), C02H(H02M), C02J(H02Q), C2(H2), C3(H3),
 C5(H5), C6(H6), C8(H8)
2.d Idealised Me refined as rotating group:
 C02I(H02N,H02O,H02P), C02K(H02R,H02S,H02T), C02L(H02U,H02V,H02W)
;
_shelx_res_checksum              58090
_shelx_hkl_checksum              9217