Dioxygen Reactivity of Biomimetic Fe(II) Complexes with Noninnocent Catecholate, o-Aminophenolate, and o-Phenylenediamine Ligands.
Bittner, Michael M.; Lindeman, Sergey V.; Popescu, Codrina V.; Fiedler, Adam T.; Inorganic chemistry 53 (2014) 4047–4061; doi:10.1021/ic403126p

data_4338054
_publ_section_title
;
 Dioxygen Reactivity of Biomimetic Fe(II) Complexes with Noninnocent
 Catecholate, o-Aminophenolate, and o-Phenylenediamine Ligands.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4047
_journal_page_last               4061
_journal_paper_doi               10.1021/ic403126p
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C56 H48 Fe N6 O2 P, C F3 O3 S, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C58.5 H51 Cl3 F3 Fe N6 O5 P S'
_chemical_formula_weight         1200.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                97.7901(14)
_cell_angle_beta                 91.8278(12)
_cell_angle_gamma                115.8745(17)
_cell_formula_units_Z            4
_cell_length_a                   15.5548(2)
_cell_length_b                   17.2278(3)
_cell_length_c                   23.4768(4)
_cell_measurement_reflns_used    40695
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4910
_cell_measurement_theta_min      3.5990
_cell_volume                     5578.95(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0622476000
_diffrn_orient_matrix_UB_12      -0.0383733000
_diffrn_orient_matrix_UB_13      -0.0585377000
_diffrn_orient_matrix_UB_21      -0.0090402000
_diffrn_orient_matrix_UB_22      0.0856299000
_diffrn_orient_matrix_UB_23      0.0004186000
_diffrn_orient_matrix_UB_31      0.0910379000
_diffrn_orient_matrix_UB_32      0.0367873000
_diffrn_orient_matrix_UB_33      -0.0317185000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            71466
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         73.72
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.654
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2476
_exptl_crystal_size_max          0.2687
_exptl_crystal_size_mid          0.2386
_exptl_crystal_size_min          0.1584
_refine_diff_density_max         1.227
_refine_diff_density_min         -0.905
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1607
_refine_ls_number_reflns         21895
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+3.0583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                19602
_reflns_number_total             21895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403126p_si_002.cif
_cod_data_source_block           '[5]OTf'
_cod_depositor_comments
'Adding full bibliography for 4338051--4338054.cif.'
_cod_original_cell_volume        5578.93(16)
_cod_original_formula_sum        'C58.50 H51 Cl3 F3 Fe N6 O5 P S'
_cod_database_code               4338054
_chemical_oxdiff_formula         'Fe C58 H48 N6 O5 S F3 P (C H2 Cl2)1.5 '
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Rigid bond restraints
 S1, F1, F2, F3, O1S, O2S, O3S, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 S1X, F1X, F2X, F3X, O1X, O2X, O3X, C57X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13X, C14X, C15X, C16X, C17X, C18X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37A, C38A, C39A, C40A, C41A, C42A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C37X, C38X, C39X, C40X, C41X, C42X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Same fragment restrains
{C13, C14, C15, C16, C17, C18}
as
{C13X, C14X, C15X, C16X, C17X, C18X}
{C37A, C38A, C39A, C40A, C41A, C42A}
as
{C37X, C38X, C39X, C40X, C41X, C42X}
{S1, F1, F2, F3, O1S, O2S, O3S, C57}
as
{S1X, F1X, F2X, F3X, O1X, O2X, O3X, C57X}
4. Others
 Sof(S1X)=Sof(F1X)=Sof(F2X)=Sof(F3X)=Sof(O1X)=Sof(O2X)=Sof(O3X)=Sof(C57X)=1-
 FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O1S)=Sof(O2S)=Sof(O3S)=Sof(C57)=FVAR(1)
 Sof(C13X)=Sof(C14X)=Sof(H14X)=Sof(C15X)=Sof(H15X)=Sof(C16X)=Sof(H16X)=
 Sof(C17X)=Sof(H17X)=Sof(C18X)=Sof(H18X)=1-FVAR(2)
 Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17)=Sof(C18)=Sof(H18)=FVAR(2)
 Sof(C37X)=Sof(C38X)=Sof(H38X)=Sof(C39X)=Sof(H39X)=Sof(C40X)=Sof(H40X)=
 Sof(C41X)=Sof(H41X)=Sof(C42X)=Sof(H42X)=1-FVAR(3)
 Sof(C37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40A)=
 Sof(C41A)=Sof(H41A)=Sof(C42A)=Sof(H42A)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
5.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C14X(H14X), C15X(H15X),
 C16X(H16X), C17X(H17X), C18X(H18X), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
 C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52),
  C54(H54), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A),
 C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C26A(H26A),
 C27A(H27A), C28A(H28A), C29A(H29A), C30A(H30A), C32A(H32A), C33A(H33A),
 C34A(H34A), C35A(H35A), C36A(H36A), C38A(H38A), C39A(H39A), C40A(H40A),
 C41A(H41A), C42A(H42A), C38X(H38X), C39X(H39X), C40X(H40X), C41X(H41X),
 C42X(H42X), C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A),
 C51A(H51A), C52A(H52A), C54A(H54A)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C55(H55A,H55B,H55C),
 C56(H56A,H56B,H56C), C4A(H4AA,H4AB,H4AC), C8A(H8AA,H8AB,H8AC), C12A(H12D,H12E,
 H12F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F)
;