Characterization of Iron-Imido Species Relevant for N-Group Transfer Chemistry.
Iovan, Diana A.; Betley, Theodore A.; Journal of the American Chemical Society 138 (2016) 1983–1993; doi:10.1021/jacs.5b12582

data_4130005
_publ_section_title
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 Characterization of Iron-Imido Species Relevant for N-Group Transfer
 Chemistry.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1983
_journal_page_last               1993
_journal_paper_doi               10.1021/jacs.5b12582
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C39 H33 Cl2 F12 Fe N4'
_chemical_formula_sum            'C39 H33 Cl2 F12 Fe N4'
_chemical_formula_weight         912.44
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                73.913(2)
_cell_angle_beta                 88.916(2)
_cell_angle_gamma                85.031(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6153(11)
_cell_length_b                   11.8003(10)
_cell_length_c                   16.1066(15)
_cell_measurement_reflns_used    4681
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.19
_cell_volume                     2113.2(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.01
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0617
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17292
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.129
_diffrn_reflns_theta_max         25.129
_diffrn_reflns_theta_min         1.316
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple-green
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         7449
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0590P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4851
_reflns_number_total             7449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           tbulfe(nhar-cf3)2
_cod_database_code               4130005
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.876
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C01K-F2 \\sim C01K-F3 \\sim C01K-F1 \\sim C01K-F1A \\sim C01K-F2A \\sim
C01K-F3A
 with sigma of 0.02
 C1-F4 \\sim C1-F5 \\sim C1-F6 \\sim C1-F4A \\sim C1-F5A \\sim C1-F6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F1A)
Uanis(F2) = Uanis(F2A)
Uanis(F3) = Uanis(F3A)
Uanis(F3) = Uanis(F1)
Uanis(F2) = Uanis(F1)
Uanis(F5) = Uanis(F4)
Uanis(F6) = Uanis(F4)
Uanis(F6A) = Uanis(F5A)
Uanis(F4A) = Uanis(F4)
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00N(H00N), C00V(H00V), C00X(H00X), C00Y(H00Y), C011(H011),
 C013(H013), C014(H014), C018(H018), C01A(H01G), C01B(H01H), C01E(H01L),
 C01F(H01M)
5.b Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C016(H01D,H01E,H01F), C01D(H01I,H01J,H01K), C01I(H01N,
 H01O,H01P), C01J(H01Q,H01R,H01S), C01M(H01T,H01U,H01V)
;
_shelx_res_checksum              46640
_shelx_hkl_checksum              60431
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'