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_4348244
_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         'C26 H26 Fe N6, 2(Cl O4), 3(C2 H3 N)'
_chemical_formula_sum            'C32 H35 Cl2 Fe N9 O8'
_chemical_formula_weight         800.44
_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
_atom_sites_solution_primary     direct
_audit_creation_date
;
'Fri Feb 21 11:43:17 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                90.0
_cell_angle_beta                 135.6985(41)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.9962(6)
_cell_length_b                   23.5193(11)
_cell_length_c                   17.3109(8)
_cell_measurement_reflns_used    5595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9950
_cell_measurement_theta_min      4.0300
_cell_volume                     3695.6(4)
_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)'
_computing_structure_solution    'ShelXS (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 0.996
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
  1 omega    5.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039   57.0000   30.0000 28

  2 omega   53.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       11.7039   57.0000   30.0000 26

  3 omega  -16.00   21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382  -99.0000 -180.0000 37

  4 omega  -39.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382   77.0000  -90.0000 93

  5 omega  -86.00  -17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9382  -38.0000  150.0000 69
;
_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      0.0391488000
_diffrn_orient_matrix_UB_12      0.0102357000
_diffrn_orient_matrix_UB_13      0.0380236000
_diffrn_orient_matrix_UB_21      -0.0172672000
_diffrn_orient_matrix_UB_22      0.0282721000
_diffrn_orient_matrix_UB_23      -0.0108325000
_diffrn_orient_matrix_UB_31      -0.0401430000
_diffrn_orient_matrix_UB_32      -0.0021906000
_diffrn_orient_matrix_UB_33      0.0377444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23625
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.705
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64007
_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            red
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          .32
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0816
_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^)+(0.0973P)^2^+6.3526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2055
_refine_ls_wR_factor_ref         0.2329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5859
_reflns_number_total             8859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01089_si_002.cif
_cod_data_source_block           bob07
_cod_original_cell_volume        3695.6(3)
_cod_original_sg_symbol_H-M      'P 1 2/c 1'
_cod_database_code               4348244
_shelxl_version_number           2013-4
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N9) = Uanis(C31)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C13(H13A,H13B), C19(H19A,H19B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24)
3.d Idealised Me refined with riding coordinates:
 C28(H28A,H28B,H28C)
3.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'