A nonheme peroxo-diiron(III) complex exhibiting both nucleophilic and electrophilic oxidation of organic substrates.
Török, Patrik; Unjaroen, Duenpen; Viktória Csendes, Flóra; Giorgi, Michel; Browne, Wesley R.; Kaizer, József; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7181–7185; doi:10.1039/d1dt01502h

data_7707397
_publ_section_title
;
 A nonheme peroxo-diiron(III) complex exhibiting both nucleophilic and
 electrophilic oxidation of organic substrates.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7181
_journal_page_last               7185
_journal_paper_doi               10.1039/d1dt01502h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C30 H21 Fe N9 S3, 2(Cl O4), C2 H3 N, H2 O'
_chemical_formula_sum            'C32 H26 Cl2 Fe N10 O9 S3'
_chemical_formula_weight         917.56
_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   mixed
_audit_creation_date             2021-01-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-01-04 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                86.615(8)
_cell_angle_beta                 80.055(9)
_cell_angle_gamma                74.102(8)
_cell_formula_units_Z            2
_cell_length_a                   11.6635(11)
_cell_length_b                   12.2558(12)
_cell_length_c                   14.2597(15)
_cell_measurement_reflns_used    2993
_cell_measurement_temperature    295
_cell_measurement_theta_max      72.5160
_cell_measurement_theta_min      4.6620
_cell_volume                     1930.8(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3048
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -96.00   -2.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.2646  125.0000 -120.0000 94

  2 omega -113.00  -10.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.2646  -57.0000   90.0000 103

  3 omega  -50.00   36.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.2646   38.0000 -120.0000 86

  4 omega  -48.00   31.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.2646   38.0000   30.0000 79

  5 omega   83.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719   45.0000 -120.0000 95

  6 omega   53.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719  -45.0000   60.0000 45

  7 omega   52.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719   15.0000    0.0000 125

  8 omega   31.00  109.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719  -94.0000  120.0000 78

  9 omega   33.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719  -45.0000  -60.0000 64

 10 omega   35.00  121.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719 -125.0000    0.0000 86

 11 omega  101.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719  125.0000 -180.0000 77

 12 omega   33.00  135.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6719  -61.0000  150.0000 102
;
_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      -0.0372851000
_diffrn_orient_matrix_UB_12      0.0866047000
_diffrn_orient_matrix_UB_13      -0.0794131000
_diffrn_orient_matrix_UB_21      -0.0631170000
_diffrn_orient_matrix_UB_22      0.0914912000
_diffrn_orient_matrix_UB_23      0.0754464000
_diffrn_orient_matrix_UB_31      0.1183327000
_diffrn_orient_matrix_UB_32      0.0348456000
_diffrn_orient_matrix_UB_33      -0.0058171000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9845
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        65.084
_diffrn_reflns_theta_max         65.084
_diffrn_reflns_theta_min         3.750
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.500
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45504
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       plate
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1404
_refine_ls_R_factor_gt           0.0867
_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^)+(0.0727P)^2^+8.5562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1993
_refine_ls_wR_factor_ref         0.2325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3854
_reflns_number_total             6348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01502h1.cif
_cod_data_source_block           bob09
_cod_depositor_comments          'Adding full bibliography for 7707397.cif.'
_cod_database_code               7707397
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c30 h21 cl2 fe1 n9 o8 s2'
_cell_oxdiff_angle_alpha         86.615(8)
_cell_oxdiff_angle_beta          80.055(9)
_cell_oxdiff_angle_gamma         74.102(8)
_cell_oxdiff_length_a            11.6635(11)
_cell_oxdiff_length_b            12.2558(12)
_cell_oxdiff_length_c            14.2597(15)
_cell_oxdiff_measurement_reflns_used 2993
_cell_oxdiff_volume              1930.8(3)
_shelx_estimated_absorpt_t_max   0.829
_shelx_estimated_absorpt_t_min   0.356
_reflns_odcompleteness_completeness 96.00
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C23) = Uanis(C24)
3.a Riding coordinates:
 O9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N9(H9), C2(H2), C4(H4), C5(H5), C6(H6A), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C1A(H1A), C20(H20), C25(H25), C24(H24),
  C23(H23), C22(H22), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              74081
_shelx_hkl_checksum              65445
_olex2_submission_special_instructions 'No special instructions were received'