#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:31:52 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289419 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/05/1570521.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570521
loop_
_publ_author_name
'Devi, Tarali'
'Dutta, Kuheli'
'Deutscher, Jennifer'
'Mebs, Stefan'
'Kuhlmann, Uwe'
'Haumann, Michael'
'Cula, Beatrice'
'Dau, Holger'
'Hildebrandt, Peter'
'Ray, Kallol'
_publ_section_title
;
 A high-spin alkylperoxo-iron(iii) complex with cis-anionic
 ligands: implications for the superoxide reductase mechanism.
;
_journal_issue                   2
_journal_name_full               'Chemical science'
_journal_page_first              528
_journal_page_last               533
_journal_paper_doi               10.1039/d3sc05603a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C13 H25 F6 Fe N3 O7 S2'
_chemical_formula_sum            'C13 H25 F6 Fe N3 O7 S2'
_chemical_formula_weight         569.33
_chemical_properties_physical    Air-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-22 deposited with the CCDC.	2023-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.662(2)
_cell_length_b                   8.8757(6)
_cell_length_c                   15.3809(9)
_cell_measurement_reflns_used    7055
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.36
_cell_volume                     4868.4(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23549
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.392
_diffrn_reflns_theta_min         2.284
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       needle
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0293P)²+7.0943P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3179
_reflns_number_total             4478
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc05603a2.cif
_cod_data_source_block           jd419_sq
_cod_depositor_comments          'Adding full bibliography for 1570521.cif.'
_cod_original_cell_volume        4868.5(5)
_cod_database_code               1570521
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.941
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe 0.36048(2) 0.31551(5) 0.22644(3) 0.01172(12) Uani 1 1 d . . . . .
F1 F 0.46007(6) 0.4694(3) 0.33357(17) 0.0558(7) Uani 1 1 d . . . . .
O1 O 0.41678(8) 0.1701(3) 0.46935(17) 0.0516(8) Uani 1 1 d . . . . .
S1 S 0.41178(2) 0.29034(11) 0.41001(5) 0.0248(2) Uani 1 1 d . . . . .
C1 C 0.31702(9) 0.5577(4) 0.3270(2) 0.0225(8) Uani 1 1 d . . . . .
H1A H 0.309531 0.662548 0.336938 0.034 Uiso 1 1 calc R U . . .
H1B H 0.331977 0.522135 0.376330 0.034 Uiso 1 1 calc R U . . .
H1C H 0.294587 0.494792 0.321003 0.034 Uiso 1 1 calc R U . . .
N1 N 0.33972(7) 0.5482(3) 0.24607(16) 0.0151(6) Uani 1 1 d . . . . .
S2 S 0.30971(2) 0.04912(9) 0.33104(5) 0.01594(19) Uani 1 1 d . . . . .
F2 F 0.47952(6) 0.2449(3) 0.35105(15) 0.0499(7) Uani 1 1 d . . . . .
O2 O 0.39390(7) 0.4234(3) 0.44269(17) 0.0451(8) Uani 1 1 d . . . . .
C2 C 0.27966(9) 0.2934(4) 0.1407(2) 0.0231(8) Uani 1 1 d . . . . .
H2A H 0.263718 0.310368 0.089690 0.035 Uiso 1 1 calc R U . . .
H2B H 0.271163 0.357675 0.188596 0.035 Uiso 1 1 calc R U . . .
H2C H 0.278046 0.187472 0.158192 0.035 Uiso 1 1 calc R U . . .
N2 N 0.31907(7) 0.3309(3) 0.11874(16) 0.0158(6) Uani 1 1 d . . . . .
C3 C 0.38944(10) 0.0231(4) 0.1487(2) 0.0260(9) Uani 1 1 d . . . . .
H3A H 0.363329 -0.011005 0.146422 0.039 Uiso 1 1 calc R U . . .
H3B H 0.399493 0.006108 0.207228 0.039 Uiso 1 1 calc R U . . .
H3C H 0.404363 -0.033426 0.106343 0.039 Uiso 1 1 calc R U . . .
N3 N 0.39117(7) 0.1853(3) 0.12803(16) 0.0165(6) Uani 1 1 d . . . . .
O3 O 0.39927(6) 0.2457(3) 0.32381(13) 0.0199(5) Uani 1 1 d . . . . .
F3 F 0.47717(6) 0.3932(3) 0.45961(14) 0.0534(7) Uani 1 1 d . . . . .
F4 F 0.30877(6) 0.1701(2) 0.48595(12) 0.0336(5) Uani 1 1 d . . . . .
O4 O 0.32254(6) 0.1939(2) 0.29718(14) 0.0195(5) Uani 1 1 d . . . . .
C4 C 0.31631(10) 0.5929(4) 0.1698(2) 0.0228(8) Uani 1 1 d . . . . .
H4A H 0.322702 0.697304 0.152753 0.027 Uiso 1 1 calc R U . . .
H4AB H 0.289536 0.591060 0.186747 0.027 Uiso 1 1 calc R U . . .
O5 O 0.33883(6) -0.0470(3) 0.36273(14) 0.0246(6) Uani 1 1 d . . . . .
F5 F 0.26733(5) -0.0023(2) 0.46635(12) 0.0298(5) Uani 1 1 d . . . . .
C5 C 0.32210(10) 0.4892(4) 0.0923(2) 0.0217(8) Uani 1 1 d . . . . .
H5A H 0.303032 0.511501 0.047337 0.026 Uiso 1 1 calc R U . . .
H5AB H 0.347171 0.507603 0.066801 0.026 Uiso 1 1 calc R U . . .
F6 F 0.25972(5) 0.2161(2) 0.40973(13) 0.0329(5) Uani 1 1 d . . . . .
O6 O 0.28125(7) -0.0196(3) 0.27852(15) 0.0289(6) Uani 1 1 d . . . . .
C6 C 0.33164(9) 0.2258(4) 0.0497(2) 0.0226(8) Uani 1 1 d . . . . .
H6A H 0.320979 0.258769 -0.006627 0.027 Uiso 1 1 calc R U . . .
H6AB H 0.321719 0.124002 0.062387 0.027 Uiso 1 1 calc R U . . .
C7 C 0.37365(10) 0.2171(4) 0.0416(2) 0.0245(8) Uani 1 1 d . . . . .
H7A H 0.380446 0.136369 0.000091 0.029 Uiso 1 1 calc R U . . .
H7AB H 0.383386 0.313675 0.018611 0.029 Uiso 1 1 calc R U . . .
O008 O 0.40530(6) 0.4603(2) 0.18098(14) 0.0197(5) Uani 1 1 d . . . . .
C8 C 0.43087(9) 0.2341(4) 0.1288(2) 0.0230(8) Uani 1 1 d . . . . .
H8A H 0.444087 0.189419 0.078366 0.028 Uiso 1 1 calc R U . . .
H8AB H 0.443144 0.197107 0.182410 0.028 Uiso 1 1 calc R U . . .
C9 C 0.43392(9) 0.4043(4) 0.1247(2) 0.0218(8) Uani 1 1 d . . . . .
H9A H 0.458955 0.437861 0.144720 0.026 Uiso 1 1 calc R U . . .
H9AB H 0.429971 0.440546 0.064541 0.026 Uiso 1 1 calc R U . . .
C10 C 0.40146(10) 0.6199(4) 0.1864(2) 0.0231(8) Uani 1 1 d . . . . .
H10A H 0.392602 0.661705 0.130340 0.028 Uiso 1 1 calc R U . . .
H10B H 0.425737 0.667372 0.201327 0.028 Uiso 1 1 calc R U . . .
C11 C 0.37310(9) 0.6470(4) 0.2568(2) 0.0223(8) Uani 1 1 d . . . . .
H11A H 0.384754 0.627480 0.314138 0.027 Uiso 1 1 calc R U . . .
H11B H 0.365093 0.753804 0.255375 0.027 Uiso 1 1 calc R U . . .
C12 C 0.45954(10) 0.3531(5) 0.3883(2) 0.0315(10) Uani 1 1 d . . . . .
C13 C 0.28509(9) 0.1120(4) 0.4281(2) 0.0204(8) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Fe01 O3 84.37(8) . . ?
O4 Fe01 O008 166.67(9) . . ?
O3 Fe01 O008 85.44(8) . . ?
O4 Fe01 N3 114.75(10) . . ?
O3 Fe01 N3 90.45(9) . . ?
O008 Fe01 N3 73.87(9) . . ?
O4 Fe01 N1 101.46(9) . . ?
O3 Fe01 N1 113.11(9) . . ?
O008 Fe01 N1 74.78(9) . . ?
N3 Fe01 N1 138.69(10) . . ?
O4 Fe01 N2 89.39(9) . . ?
O3 Fe01 N2 166.58(9) . . ?
O008 Fe01 N2 102.30(9) . . ?
N3 Fe01 N2 81.37(9) . . ?
N1 Fe01 N2 79.76(9) . . ?
O1 S1 O2 116.82(18) . . ?
O1 S1 O3 114.90(16) . . ?
O2 S1 O3 114.07(15) . . ?
O1 S1 C12 103.36(18) . . ?
O2 S1 C12 103.19(18) . . ?
O3 S1 C12 101.71(15) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 N1 C11 108.0(2) . . ?
C1 N1 C4 109.7(2) . . ?
C11 N1 C4 112.2(3) . . ?
C1 N1 Fe01 110.45(19) . . ?
C11 N1 Fe01 107.33(19) . . ?
C4 N1 Fe01 109.12(18) . . ?
O5 S2 O6 116.93(15) . . ?
O5 S2 O4 114.76(13) . . ?
O6 S2 O4 113.30(14) . . ?
O5 S2 C13 104.71(15) . . ?
O6 S2 C13 104.54(15) . . ?
O4 S2 C13 100.01(14) . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C5 N2 C6 112.4(3) . . ?
C5 N2 C2 110.4(3) . . ?
C6 N2 C2 108.0(2) . . ?
C5 N2 Fe01 102.49(19) . . ?
C6 N2 Fe01 107.10(19) . . ?
C2 N2 Fe01 116.51(19) . . ?
N3 C3 H3A 109.5 . . ?
N3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C3 N3 C8 108.9(3) . . ?
C3 N3 C7 111.0(3) . . ?
C8 N3 C7 110.6(3) . . ?
C3 N3 Fe01 110.10(19) . . ?
C8 N3 Fe01 108.51(19) . . ?
C7 N3 Fe01 107.76(19) . . ?
S1 O3 Fe01 139.53(14) . . ?
S2 O4 Fe01 149.55(15) . . ?
N1 C4 C5 112.3(3) . . ?
N1 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
N1 C4 H4AB 109.1 . . ?
C5 C4 H4AB 109.1 . . ?
H4A C4 H4AB 107.9 . . ?
N2 C5 C4 110.6(3) . . ?
N2 C5 H5A 109.5 . . ?
C4 C5 H5A 109.5 . . ?
N2 C5 H5AB 109.5 . . ?
C4 C5 H5AB 109.5 . . ?
H5A C5 H5AB 108.1 . . ?
N2 C6 C7 113.1(3) . . ?
N2 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
N2 C6 H6AB 109.0 . . ?
C7 C6 H6AB 109.0 . . ?
H6A C6 H6AB 107.8 . . ?
N3 C7 C6 110.6(3) . . ?
N3 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
N3 C7 H7AB 109.5 . . ?
C6 C7 H7AB 109.5 . . ?
H7A C7 H7AB 108.1 . . ?
C10 O008 C9 116.7(2) . . ?
C10 O008 Fe01 119.99(18) . . ?
C9 O008 Fe01 121.10(19) . . ?
N3 C8 C9 111.1(3) . . ?
N3 C8 H8A 109.4 . . ?
C9 C8 H8A 109.4 . . ?
N3 C8 H8AB 109.4 . . ?
C9 C8 H8AB 109.4 . . ?
H8A C8 H8AB 108.0 . . ?
O008 C9 C8 105.7(3) . . ?
O008 C9 H9A 110.6 . . ?
C8 C9 H9A 110.6 . . ?
O008 C9 H9AB 110.6 . . ?
C8 C9 H9AB 110.6 . . ?
H9A C9 H9AB 108.7 . . ?
O008 C10 C11 105.4(3) . . ?
O008 C10 H10A 110.7 . . ?
C11 C10 H10A 110.7 . . ?
O008 C10 H10B 110.7 . . ?
C11 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
N1 C11 C10 111.3(3) . . ?
N1 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
N1 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
F3 C12 F2 107.4(3) . . ?
F3 C12 F1 108.1(3) . . ?
F2 C12 F1 106.3(3) . . ?
F3 C12 S1 112.1(3) . . ?
F2 C12 S1 111.1(3) . . ?
F1 C12 S1 111.5(3) . . ?
F6 C13 F4 107.8(3) . . ?
F6 C13 F5 107.5(3) . . ?
F4 C13 F5 107.5(3) . . ?
F6 C13 S2 111.7(2) . . ?
F4 C13 S2 111.2(2) . . ?
F5 C13 S2 111.0(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 O4 2.045(2) . ?
Fe01 O3 2.131(2) . ?
Fe01 O008 2.167(2) . ?
Fe01 N3 2.196(3) . ?
Fe01 N1 2.214(3) . ?
Fe01 N2 2.223(3) . ?
F1 C12 1.331(4) . ?
O1 S1 1.415(3) . ?
S1 O2 1.434(3) . ?
S1 O3 1.454(2) . ?
S1 C12 1.823(4) . ?
C1 N1 1.487(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
N1 C11 1.488(4) . ?
N1 C4 1.494(4) . ?
S2 O5 1.430(2) . ?
S2 O6 1.433(2) . ?
S2 O4 1.460(2) . ?
S2 C13 1.819(3) . ?
F2 C12 1.326(4) . ?
C2 N2 1.483(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
N2 C5 1.467(4) . ?
N2 C6 1.483(4) . ?
C3 N3 1.476(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
N3 C8 1.480(4) . ?
N3 C7 1.496(4) . ?
F3 C12 1.314(4) . ?
F4 C13 1.331(4) . ?
C4 C5 1.519(5) . ?
C4 H4A 0.9900 . ?
C4 H4AB 0.9900 . ?
F5 C13 1.333(4) . ?
C5 H5A 0.9900 . ?
C5 H5AB 0.9900 . ?
F6 C13 1.323(4) . ?
C6 C7 1.505(5) . ?
C6 H6A 0.9900 . ?
C6 H6AB 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7AB 0.9900 . ?
O008 C10 1.425(4) . ?
O008 C9 1.428(4) . ?
C8 C9 1.516(5) . ?
C8 H8A 0.9900 . ?
C8 H8AB 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9AB 0.9900 . ?
C10 C11 1.502(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
