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_4130004
_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 Cl4 Fe N2'
_chemical_formula_sum            'C23 H25 Cl4 Fe N2'
_chemical_formula_weight         527.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 126.613(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.064(2)
_cell_length_b                   17.537(3)
_cell_length_c                   11.077(3)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.09
_cell_measurement_theta_min      2.20
_cell_volume                     2348.9(8)
_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      99.99
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17698
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.204
_diffrn_reflns_theta_max         25.204
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.111
_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    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4189
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0167P)^2^+0.0073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0478
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                3911
_reflns_number_total             4189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           tbulfecl2
_cod_original_cell_volume        2348.8(8)
_cod_database_code               4130004
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.718
_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:
 C008(H008), C00C(H00C), C00E(H00E), C00I(H00I), C00J(H00J), C00R(H00T),
 C00T(H00X)
2.b Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00D), C00L(H00F,H00G,H00H), C00N(H00K,H00L,H00M), C00O(H00N,
 H00O,H00P), C00P(H00Q,H00R,H00S), C00S(H00U,H00V,H00W)
;
_shelx_res_checksum              6612
_shelx_hkl_checksum              95326
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'