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_4130001
_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         '2(C31 H30 Cl3 F6 Fe N3), 0.5(C6 H6)'
_chemical_formula_sum            'C65 H63 Cl6 F12 Fe2 N6'
_chemical_formula_weight         1480.61
_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   mixed
_audit_creation_date             2015-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.3970(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6061(6)
_cell_length_b                   31.1222(14)
_cell_length_c                   17.3548(7)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.30
_cell_volume                     7148.9(5)
_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      99.98
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0893
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54141
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.222
_diffrn_reflns_theta_max         25.222
_diffrn_reflns_theta_min         2.162
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green-red
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.570
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         12782
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0784
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+27.4622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8012
_reflns_number_total             12782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12582_si_002.cif
_cod_data_source_block           tbulfeclnh2ar-cf3
_cod_database_code               4130001
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C02F-F1A \\sim C02F-F1B \\sim C02F-F2A \\sim C02F-F2B \\sim C02F-F3A \\sim
C02F-F3B
 with sigma of 0.02
 N00K-H00D \\sim N00K-H00C
 with sigma of 0.02
3. Rigid bond restraints
 C01S, C02E
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C01S, C02H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C01S \\sim C02E: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C01S \\sim C02H: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Cl3) = Uanis(Cl3A)
Uanis(F00V) = Uanis(F00W)
Uanis(F00Y) = Uanis(F00Z)
Uanis(F00J) = Uanis(F00K)
Uanis(C6) = Uanis(C3) = Uanis(C1) = Uanis(C2) = Uanis(C8) = Uanis(C7)
Uanis(C02H) = Uanis(C02E)
Uanis(F1A) = Uanis(F00C)
Uanis(F2A) = Uanis(F00B)
Uanis(F3A) = Uanis(F00A)
Uanis(F1B) = Uanis(F00C)
Uanis(F2B) = Uanis(F00B)
Uanis(F3B) = Uanis(F00A)
5. Others
 Sof(Cl3A)=1-FVAR(1)
 Sof(Cl3)=FVAR(1)
 Sof(F00W)=Sof(F00Z)=Sof(F00K)=1-FVAR(2)
 Sof(F00J)=Sof(F00V)=Sof(F00Y)=FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(3)
 Sof(F2A)=Sof(F3A)=Sof(F1A)=FVAR(3)
 Fixed Sof: C6(0.5) H6(0.5) C1(0.5) H1(0.5) C3(0.5) H3(0.5) C2(0.5) H2(0.5)
 C8(0.5) H8(0.5) C7(0.5) H7(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N00L(H00A,H00B)
6.b Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C011(H011), C012(H012), C013(H013), C014(H014), C015(H015),
 C017(H017), C018(H018), C01C(H01C), C01E(H01E), C01F(H01N), C01G(H01G),
 C01H(H01O), C01I(H01I), C01P(H01P), C025(H025), C026(H026), C02B(H02P),
 C02C(H02Q), C02D(H02R), C6(H6), C1(H1), C3(H3), C2(H2), C8(H8), C7(H7)
6.c Fitted hexagon refined as free rotating group:
 C6(C1,C3,C2,C8,C7)
6.d Idealised Me refined as rotating group:
 C01M(H01A,H01B,H01D), C01T(H01F,H01H,H01J), C01V(H01Q,H01R,H01S), C01W(H01T,
 H01U,H01V), C01X(H01W,H01X,H01Y), C01Y(H01K,H01L,H01M), C024(H02A,H02B,H02C),
 C027(H02J,H02K,H02L), C02A(H02M,H02N,H02O), C02E(H02D,H02E,H02F), C02G(H02S,
 H02T,H02U), C02H(H02G,H02H,H02I)
;
_shelx_res_checksum              18685
_shelx_hkl_checksum              89139
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'