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_4130000
_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         'C54 H53 Cl6 F6 Fe2 N5, 0.5(C6 H6)'
_chemical_formula_sum            'C57 H56 Cl6 F6 Fe2 N5'
_chemical_formula_weight         1249.46
_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             2015-08-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                96.7240(13)
_cell_angle_beta                 96.7310(13)
_cell_angle_gamma                113.9150(12)
_cell_formula_units_Z            2
_cell_length_a                   12.7480(9)
_cell_length_b                   13.0508(9)
_cell_length_c                   19.9343(13)
_cell_measurement_reflns_used    7033
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.18
_cell_volume                     2961.0(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      100.01
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0657
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29648
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.222
_diffrn_reflns_theta_max         25.222
_diffrn_reflns_theta_min         1.046
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.820
_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    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.098
_refine_diff_density_max         1.893
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         10580
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0614
_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^)+(0.1088P)^2^+1.1487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6981
_reflns_number_total             10580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           bis-fecl_imido
_cod_database_code               4130000
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.834
_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
 C1S-C2S \\sim C2S-C3S \\sim C3S-C4S \\sim C4S-C5S \\sim C5S-C6S \\sim C6S-C1S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) = Uanis(C01X)
Uanis(C2S) = Uanis(C01Y)
Uanis(C3S) = Uanis(C019)
Uanis(C4S) = Uanis(C00K)
Uanis(C5S) = Uanis(C01J)
Uanis(C6S) = Uanis(C01M)
4. Others
 Fixed Sof: C5S(0.5) H5S(0.5) C3S(0.5) H3S(0.5) C2S(0.5) H2S(0.5) C4S(0.5)
 H4S(0.5) C6S(0.5) H6S(0.5) C1S(0.5) H1S(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00U(H00U), C011(H011), C012(H012), C013(H013), C018(H018),
 C01B(H01D), C01C(H01E), C01E(H01F), C01F(H01G), C01G(H01H), C01M(H01O),
 C01P(H01S), C01U(H01Z), C01V(H01), C01X(H1AA), C01Y(H2AA), C5S(H5S), C3S(H3S),
 C2S(H2S), C4S(H4S), C6S(H6S), C1S(H1S)
5.b Idealised Me refined as rotating group:
 C00V(H00A,H00B,H00C), C00Z(H00D,H00E,H00F), C01A(H01A,H01B,H01C), C01H(H01I,
 H01J,H01K), C01I(H01L,H01M,H01N), C01O(H01P,H01Q,H01R), C01R(H01T,H01U,H01V),
 C01S(H01W,H01X,H01Y), C01W(H0AA,H,HA), C01Z(H3AA,HB,HC), C020(H02A,H02B,H02C),
 C021(H02D,H02E,H02F)
;
_shelx_res_checksum              83471
_shelx_hkl_checksum              756
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'