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_4130003
_publ_section_title
;
 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         'C31 H29 Cl3 F6 Fe N3, 2(C3 H3)'
_chemical_formula_sum            'C37 H35 Cl3 F6 Fe N3'
_chemical_formula_weight         797.88
_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
_audit_creation_date             2015-08-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                76.462(4)
_cell_angle_beta                 82.700(4)
_cell_angle_gamma                71.185(4)
_cell_formula_units_Z            2
_cell_length_a                   12.267(4)
_cell_length_b                   12.613(4)
_cell_length_c                   13.807(4)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.26
_cell_volume                     1962.8(11)
_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      100.03
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_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  0.0864
_diffrn_reflns_av_unetI/netI     0.1369
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11840
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.519
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       plate
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1692
_refine_ls_R_factor_gt           0.0923
_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^)+(0.1703P)^2^+0.1095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2581
_refine_ls_wR_factor_ref         0.3026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3500
_reflns_number_total             6590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           tbulfeclnhar_cf3
_cod_database_code               4130003
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.860
_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
 N00D-H00D
 1.05 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C5) = Uanis(C3) = Uanis(C4) = Uanis(C1) = Uanis(C2)
Uanis(C00M) = Uanis(C00H)
4. Others
 Fixed Sof: C1(0.5) H1(0.5) C4(0.5) H4(0.5) C3(0.5) H3(0.5) C5(0.5) H5(0.5)
 C6(0.5) H6(0.5) C2(0.5) H2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00J(H00J), C00L(H00L), C00P(H00P), C00Q(H00Q), C00S(H00S),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C019(H019), C01A(H01S),
 C01B(H01T), C1(H1), C4(H4), C3(H3), C5(H5), C6(H6), C2(H2)
5.b Fitted hexagon refined as free rotating group:
 C1(C4,C3,C5,C6,C2)
5.c Idealised Me refined as rotating group:
 C010(H01A,H01B,H01C), C012(H01D,H01E,H01F), C013(H01G,H01H,H01I), C014(H01J,
 H01K,H01L), C015(H01M,H01N,H01O), C018(H01P,H01Q,H01R)
;
_shelx_res_checksum              95246
_shelx_hkl_checksum              35607
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'