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_4131546
_publ_section_title
;
 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         'C75 H60 Fe N3, 2(C5 H10)'
_chemical_formula_sum            'C85 H80 Fe N3'
_chemical_formula_weight         1199.37
_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             2015-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                87.8430(10)
_cell_angle_beta                 72.1640(10)
_cell_angle_gamma                82.1700(10)
_cell_formula_units_Z            2
_cell_length_a                   13.4127(9)
_cell_length_b                   15.9534(10)
_cell_length_c                   16.6919(11)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.06
_cell_measurement_theta_min      2.34
_cell_volume                     3368.3(4)
_computing_cell_refinement       'SAINT 8.43A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX2 v2014.3.0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT 8.43A (Bruker-AXS, 2014)'
_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      100.03
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37031
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.282
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.367
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         11944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0777P)^2^+4.9012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9466
_reflns_number_total             11944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06682_si_002.cif
_cod_data_source_block           ArLFeNMes
_cod_database_code               4131546
_shelxl_version_number           2014/6
_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 Secondary CH2 refined with riding coordinates:
 C02B(H02G,H02H), C02C(H02P,H02Q), C02D(H02R,H02S)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00G(H00G), C00K(H00K), C00L(H00L), C00M(H00M), C00P(H00P),
 C00R(H00R), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X), C010(H010),
 C011(H011), C012(H012), C015(H015), C016(H016), C018(H018), C01A(H01A),
 C01C(H01C), C01D(H01D), C01E(H01E), C01G(H01G), C01H(H01H), C01I(H01I),
 C01J(H01J), C01K(H01K), C01M(H01M), C01N(H01N), C01P(H01P), C01Q(H01Q),
 C01R(H01R), C01V(H01Z), C01W(H01), C01Y(H1AA), C01Z(H2AA), C020(H020),
 C021(H021), C022(H022), C023(H023), C025(H025), C026(H026), C027(H027),
 C029(H029), C02F(H02L), C02H(H02V)
2.c X=CH2 refined with riding coordinates:
 C02G(H02T,H02U)
2.d Idealised Me refined as rotating group:
 C01O(H01B,H01F,H01L), C01S(H01O,H01S,H01T), C01T(H01U,H01V,H01W), C01U(H01X,
 H01Y,H), C01X(H0AA,HA,HB), C024(H02A,H02B,H02C), C028(H02D,H02E,H02F),
 C02A(H02M,H02N,H02O), C02E(H02I,H02J,H02K)
;
_shelx_res_checksum              72907
_shelx_hkl_checksum              76181