Formation, Characterization, and Reactivity of a Nonheme Oxoiron(IV) Complex Derived from the Chiral Pentadentate Ligand asN4Py.
Lakk-Bogáth, Dóra; Csonka, Róbert; Speier, Gábor; Réglier, Marius; Simaan, A. Jalila; Naubron, Jean-Valère; Giorgi, Michel; Lázár, Károly; Kaizer, József; Inorganic chemistry 55 (2016) 10090–10093; doi:10.1021/acs.inorgchem.6b01089

data_4348245
_publ_section_title
;
 Formation, Characterization, and Reactivity of a Nonheme Oxoiron(IV)
 Complex Derived from the Chiral Pentadentate Ligand asN4Py.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10090
_journal_page_last               10093
_journal_paper_doi               10.1021/acs.inorgchem.6b01089
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C24 H23 N5'
_chemical_formula_sum            'C24 H23 N5'
_chemical_formula_weight         381.47
_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
;
'Wed Mar 05 22:29:07 2014'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_cell_angle_alpha                102.349(5)
_cell_angle_beta                 104.313(6)
_cell_angle_gamma                95.215(5)
_cell_formula_units_Z            2
_cell_length_a                   8.6788(6)
_cell_length_b                   8.8994(4)
_cell_length_c                   13.9946(9)
_cell_measurement_reflns_used    3877
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4480
_cell_measurement_theta_min      4.3150
_cell_volume                     1011.24(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_details
;
  1 omega   11.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.6643 -140.0000 -168.0000 64

  2 omega  -38.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987   57.0000   30.0000 101

  3 omega  -83.00   18.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987  -57.0000 -120.0000 101

  4 omega  -20.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.6643  -99.0000 -120.0000 71

  5 omega  -20.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -        9.6643  -99.0000  -60.0000 71

  6 omega  -38.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987   57.0000 -180.0000 101

  7 omega  -38.00   63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987   57.0000  -30.0000 101

  8 omega  -20.00   31.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987  -99.0000  120.0000 51

  9 omega  -86.00   23.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8987  -77.0000   60.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0150950000
_diffrn_orient_matrix_UB_12      -0.0312094000
_diffrn_orient_matrix_UB_13      0.0399614000
_diffrn_orient_matrix_UB_21      0.0468730000
_diffrn_orient_matrix_UB_22      0.0671145000
_diffrn_orient_matrix_UB_23      0.0361636000
_diffrn_orient_matrix_UB_31      -0.0696943000
_diffrn_orient_matrix_UB_32      0.0365462000
_diffrn_orient_matrix_UB_33      -0.0024410000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20276
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.941
_diffrn_reflns_theta_min         3.384
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description
;
;
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0306P)^2^+0.2486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2876
_reflns_number_total             4686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01089_si_003.cif
_cod_data_source_block           bobligand
_cod_database_code               4348245
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'