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_4129998
_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         'C23 H25 Cl3 Fe N2, C6 H6'
_chemical_formula_sum            'C29 H31 Cl3 Fe N2'
_chemical_formula_weight         569.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 94.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4486(11)
_cell_length_b                   10.8936(9)
_cell_length_c                   18.8713(16)
_cell_measurement_reflns_used    8248
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.16
_cell_volume                     2755.4(4)
_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      99.96
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23478
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.040
_diffrn_reflns_theta_max         25.040
_diffrn_reflns_theta_min         1.792
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0349 before and 0.0300 after correction.
The Ratio of minimum to maximum transmission is 0.9410.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red-green
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0196P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3417
_reflns_number_total             4871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           tbulfecl_dimer
_cod_database_code               4129998
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.759
_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.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00H(H00H), C00I(H00I), C00K(H00K), C00M(H00Z), C00P(H00P),
 C00Q(H00Q), C00R(H00R), C00S(H00), C00U(H0AA), C00V(H1AA), C00W(H2AA),
 C00X(H3AA)
2.b Idealised Me refined as rotating group:
 C00L(H00A,H00C,H00D), C00N(H00E,H00F,H00G), C00O(H00J,H00L,H00M), C00T(H00N,
 H00O,H00S), C00Y(H00T,H00U,H00V), C00Z(H00W,H00X,H00Y)
;
_shelx_res_checksum              4358
_shelx_hkl_checksum              31574
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'