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_4129999
_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         'C35 H42 Cl3 Fe N3, C6 H5 F'
_chemical_formula_sum            'C41 H47 Cl3 F Fe N3'
_chemical_formula_weight         763.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 93.660(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1706(18)
_cell_length_b                   16.847(3)
_cell_length_c                   19.035(3)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.28
_cell_volume                     3894.9(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      100.01
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56642
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.148
_diffrn_reflns_theta_max         25.148
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.630
_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    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6907
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0779P)^2^+8.3128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5199
_reflns_number_total             6907
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           feclnphdip_iminyl
_cod_original_cell_volume        3895.0(10)
_cod_database_code               4129999
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.765
_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. Rigid bond restraints
 F1, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim C5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1A) = Uanis(C1B)
Uanis(C3A) = Uanis(C3B)
Uanis(C2A) = Uanis(C2B)
Uanis(C5) = Uanis(C6) = Uanis(C4) = Uanis(C1) = Uanis(C2) = Uanis(C3)
4. Others
 Sof(C1B)=Sof(H1B)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(C2B)=Sof(H2BA)=
 Sof(H2BB)=Sof(H2BC)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C00I(H00I), C1A(H1A), C1B(H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L), C00O(H00O),
 C00P(H00P), C00R(H00R), C00S(H00S), C00U(H00U), C6(H6), C3(H3), C2(H2), C1(H1),
  C4(H4)
5.c Fitted hexagon refined as free rotating group:
 C6(C5,C3,C2,C1,C4)
5.d Idealised Me refined as rotating group:
 C00Q(H00A,H00B,H00C), C00X(H00D,H00E,H00J), C00Y(H00M,H00N,H00Q), C00Z(H00T,
 H00V,H00W), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,H01H,H01I),
 C013(H01J,H01K,H01L), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,
 H3BC), C2B(H2BA,H2BB,H2BC)
;
_shelx_res_checksum              75469
_shelx_hkl_checksum              67887
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'