data_A
_audit_creation_date               2020-11-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

#CrysAlisPro, version 171.40.84a
Rigaku Oxford Diffraction (2020). CrysAlisPro Software system,
version 171.40.84a. Rigaku Corporation, Oxford, UK.

#SHELXT-2018/2
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3--8.

#SHELXL-2018/3
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3--8.
;
_publ_contact_author_name        'William D. Jones'
_publ_contact_author_address     
;
 'Department of Chemistry, University of Rochester, Rochester, New York 14627'
;
_publ_contact_author_email       'jones@chem.rochester.edu'
_publ_requested_journal          'J. Am. Chem. Soc.'
_publ_section_title            
;
Iron-Based Dehydration Catalyst for Selective Formation of Styrene
;

loop_
_publ_author_name                
 'Olaf Nachtigall'
 'Andrew I. VanderWeide'
 'William W. Brennessel'
 'William D. Jones'

_publ_author_address             
;
 Department of Chemistry, University of Rochester, Rochester, NY  14627 USA
;

_chemical_name_common              jonon95
_chemical_name_systematic          '(FOX)Fe(OTf)2'
_chemical_formula_moiety           'C18 H17 F6 Fe N3 O9 S2'
_chemical_formula_sum              'C18 H17 F6 Fe N3 O9 S2'
_chemical_formula_weight           653.32
_chemical_melting_point            ?
_chemical_oxdiff_formula           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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'
 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe' 'Fe' -1.1336 3.1974
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/n 1'
_space_group_name_Hall             '-P 2yn'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                     10.99030(10)
_cell_length_b                     15.5335(2)
_cell_length_c                     14.0576(2)
_cell_angle_alpha                  90
_cell_angle_beta                   99.8240(10)
_cell_angle_gamma                  90
_cell_volume                       2364.69(5)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      27130
_cell_measurement_temperature      100.01(10)
_cell_measurement_theta_max        77.5570
_cell_measurement_theta_min        4.2690
_shelx_estimated_absorpt_T_max     0.406
_shelx_estimated_absorpt_T_min     0.279
_exptl_absorpt_coefficient_mu      7.749
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.69760
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'light yellow'
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.835
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1320
_exptl_crystal_size_max            0.221
_exptl_crystal_size_mid            0.184
_exptl_crystal_size_min            0.142
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0647
_diffrn_reflns_av_unetI/netI       0.0273
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.970
_diffrn_reflns_limit_h_max         13
_diffrn_reflns_limit_h_min         -13
_diffrn_reflns_limit_k_max         19
_diffrn_reflns_limit_k_min         -19
_diffrn_reflns_limit_l_max         17
_diffrn_reflns_limit_l_min         -17
_diffrn_reflns_number              40193
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.970
_diffrn_reflns_theta_full          74.504
_diffrn_reflns_theta_max           79.787
_diffrn_reflns_theta_min           4.277
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        100.01(10)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -49.00  22.00   0.50    0.05    --  -49.75  49.00  64.00  142
  2  ω    -49.00 -12.00   0.50    0.16    --  -84.25  49.00  64.00   74
  3  ω    -42.00 -12.00   0.50    0.16    --  -84.25  45.00-120.00   60
  4  ω   -121.00 -39.00   0.50    0.05    --  -49.75 -49.00 -82.00  164
  5  ω    -21.00  60.00   0.50    0.05    --   49.75 -49.00 -82.00  162
  6  ω     34.00  61.00   0.50    0.16    --  105.75 -49.00 -82.00   54
  7  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00-120.00  106
  8  ω     98.00 164.00   0.50    0.16    --  105.75  15.00 -90.00  132
  9  ω     98.00 178.00   0.50    0.16    --  105.75  30.00   0.00  160
 10  ω     96.00 178.00   0.50    0.16    --  105.75  49.00  64.00  164
 11  ω     97.00 178.00   0.50    0.16    --  105.75  45.00 -60.00  162
 12  ω     98.00 164.00   0.50    0.16    --  105.75  15.00-180.00  132
 13  ω     92.00 178.00   0.50    0.16    --  105.75  61.00-180.00  172
 14  ω     92.00 178.00   0.50    0.16    --  105.75 125.00 -90.00  172
 15  ω     98.00 164.00   0.50    0.16    --  105.75  15.00   0.00  132
 16  ω     92.00 178.00   0.50    0.16    --  105.75 125.00 -30.00  172
 17  ω     40.00 121.00   0.50    0.05    --   49.75  49.00  64.00  162
 18  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00  60.00  106
 19  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00 150.00  106
 20  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00  90.00  106
 21  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00   0.00  106
 22  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00 -60.00  106
 23  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00-150.00  106
 24  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00-180.00  106
 25  ω     34.00  87.00   0.50    0.16    --  105.75 -61.00 -30.00  106
 26  ω     29.00 121.00   0.50    0.05    --   49.75  77.00-150.00  184
 27  ω     29.00 121.00   0.50    0.05    --   49.75  77.00 -90.00  184
 28  ω     29.00  82.00   0.50    0.05    --   49.75  77.00-180.00  106
 29  ω     29.00 121.00   0.50    0.05    --   49.75  77.00 120.00  184
 30  ω   -121.00 -70.00   0.50    0.05    --  -49.75-125.00  60.00  102
 31  ω   -121.00 -70.00   0.50    0.05    --  -49.75-125.00  30.00  102
 32  ω   -121.00 -37.00   0.50    0.05    --  -49.75 -57.00   0.00  168
 33  ω   -121.00 -70.00   0.50    0.05    --  -49.75-125.00-150.00  102
 34  ω   -156.00 -74.00   0.50    0.16    --  -84.25 -49.00 -82.00  164
 35  ω   -121.00 -29.00   0.50    0.05    --  -49.75 -77.00  90.00  184
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0570046000
_diffrn_orient_matrix_UB_12        -0.0597009000
_diffrn_orient_matrix_UB_13        -0.0832406000
_diffrn_orient_matrix_UB_21        -0.1272724000
_diffrn_orient_matrix_UB_22        0.0095589000
_diffrn_orient_matrix_UB_23        0.0307500000
_diffrn_orient_matrix_UB_31        -0.0280165000
_diffrn_orient_matrix_UB_32        0.0786870000
_diffrn_orient_matrix_UB_33        -0.0669876000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Cu K\a'
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  4757
_reflns_number_total               4997
_reflns_odcompleteness_completeness  99.94
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max           0.373
_refine_diff_density_min           -0.477
_refine_diff_density_rms           0.076
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.051
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       356
_refine_ls_number_reflns           4997
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0323
_refine_ls_R_factor_gt             0.0306
_refine_ls_restrained_S_all        1.051
_refine_ls_shift/su_max            0.002
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0426P)²+1.8932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0795
_refine_ls_wR_factor_ref           0.0812
_refine_special_details            ?
_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), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap
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
 Fe1 Fe 0.72695(2) 0.30972(2) 0.51546(2) 0.01155(8) Uani 1 1 d . . . . .
 S1 S 0.84828(4) 0.47124(3) 0.65288(3) 0.01697(11) Uani 1 1 d . . . . .
 S2 S 0.57399(4) 0.36745(3) 0.28728(3) 0.01457(10) Uani 1 1 d . . . . .
 F1 F 1.07543(12) 0.48001(9) 0.74387(9) 0.0303(3) Uani 1 1 d . . . . .
 F2 F 1.05975(11) 0.47768(8) 0.58949(9) 0.0262(3) Uani 1 1 d . . . . .
 F3 F 1.03110(12) 0.36151(8) 0.66543(10) 0.0300(3) Uani 1 1 d . . . . .
 F4 F 0.59822(12) 0.32625(9) 0.11156(8) 0.0313(3) Uani 1 1 d . . . . .
 F5 F 0.74599(13) 0.40509(10) 0.18591(10) 0.0375(3) Uani 1 1 d . . . . .
 F6 F 0.73598(12) 0.27099(9) 0.22192(9) 0.0306(3) Uani 1 1 d . . . . .
 O1 O 0.80192(13) 0.24269(9) 0.64565(10) 0.0187(3) Uani 1 1 d . . . . .
 H1 H 0.864(3) 0.2411(19) 0.685(2) 0.033(7) Uiso 1 1 d . . . . .
 O2 O 0.72832(13) 0.04199(8) 0.46581(10) 0.0197(3) Uani 1 1 d . . . . .
 O3 O 0.46493(12) 0.10456(8) 0.49957(9) 0.0167(3) Uani 1 1 d . . . . .
 O4 O 0.79691(12) 0.42869(8) 0.56182(9) 0.0184(3) Uani 1 1 d . . . . .
 O5 O 0.81303(15) 0.43280(11) 0.73677(11) 0.0304(4) Uani 1 1 d . . . . .
 O6 O 0.84401(14) 0.56306(9) 0.64617(11) 0.0268(3) Uani 1 1 d . . . . .
 O7 O 0.66419(12) 0.37720(8) 0.37518(9) 0.0169(3) Uani 1 1 d . . . . .
 O8 O 0.49783(13) 0.29137(9) 0.28679(10) 0.0213(3) Uani 1 1 d . . . . .
 O9 O 0.51079(13) 0.44486(9) 0.25290(10) 0.0239(3) Uani 1 1 d . . . . .
 N1 N 0.64853(14) 0.17682(9) 0.49497(10) 0.0129(3) Uani 1 1 d . . . . .
 N2 N 0.85450(14) 0.24825(10) 0.44002(11) 0.0144(3) Uani 1 1 d . . . . .
 N3 N 0.54117(14) 0.32510(10) 0.53978(11) 0.0146(3) Uani 1 1 d . . . . .
 C1 C 0.71640(18) 0.18241(12) 0.67410(13) 0.0174(4) Uani 1 1 d . . . . .
 H1A H 0.648485 0.212831 0.694956 0.021 Uiso 1 1 calc R U . . .
 H1B H 0.757163 0.147651 0.727494 0.021 Uiso 1 1 calc R U . . .
 C2 C 0.66774(17) 0.12489(11) 0.58778(13) 0.0147(3) Uani 1 1 d . . . . .
 C3 C 0.75879(18) 0.05588(12) 0.56777(14) 0.0196(4) Uani 1 1 d . . . . .
 H3A H 0.843269 0.075742 0.585663 0.024 Uiso 1 1 calc R U . . .
 H3B H 0.748428 0.003469 0.603045 0.024 Uiso 1 1 calc R U . . .
 C4 C 0.71009(17) 0.12569(11) 0.42728(13) 0.0154(4) Uani 1 1 d . . . . .
 H4 H 0.655076 0.122458 0.364709 0.019 Uiso 1 1 calc R U . . .
 C5 C 0.53757(17) 0.08854(12) 0.59274(13) 0.0165(4) Uani 1 1 d . . . . .
 H5A H 0.541868 0.027313 0.606438 0.020 Uiso 1 1 calc R U . . .
 H5B H 0.502128 0.117415 0.642761 0.020 Uiso 1 1 calc R U . . .
 C6 C 0.51330(17) 0.18075(11) 0.46640(13) 0.0145(3) Uani 1 1 d . . . . .
 H6 H 0.491956 0.183592 0.395883 0.017 Uiso 1 1 calc R U . . .
 C7 C 0.83244(17) 0.16596(12) 0.41273(13) 0.0147(3) Uani 1 1 d . . . . .
 C8 C 0.91210(19) 0.11936(13) 0.36592(14) 0.0210(4) Uani 1 1 d . . . . .
 H8 H 0.894907 0.062401 0.348144 0.025 Uiso 1 1 calc R U . . .
 C9 C 1.01804(19) 0.15919(14) 0.34600(15) 0.0224(4) Uani 1 1 d . . . . .
 H9 H 1.073491 0.129111 0.315358 0.027 Uiso 1 1 calc R U . . .
 C10 C 1.03987(17) 0.24463(13) 0.37257(14) 0.0194(4) Uani 1 1 d . . . . .
 H10 H 1.109356 0.273054 0.358931 0.023 Uiso 1 1 calc R U . . .
 C11 C 0.95662(17) 0.28665(12) 0.41959(13) 0.0167(4) Uani 1 1 d . . . . .
 H11 H 0.971763 0.343721 0.437837 0.020 Uiso 1 1 calc R U . . .
 C12 C 0.46300(16) 0.26035(11) 0.51058(13) 0.0142(3) Uani 1 1 d . . . . .
 C13 C 0.33798(17) 0.26476(13) 0.51483(14) 0.0185(4) Uani 1 1 d . . . . .
 H13 H 0.286244 0.218352 0.495353 0.022 Uiso 1 1 calc R U . . .
 C14 C 0.29162(18) 0.33965(13) 0.54863(14) 0.0205(4) Uani 1 1 d . . . . .
 H14 H 0.207860 0.344546 0.551021 0.025 Uiso 1 1 calc R U . . .
 C15 C 0.37131(18) 0.40711(13) 0.57882(15) 0.0205(4) Uani 1 1 d . . . . .
 H15 H 0.342188 0.457938 0.601751 0.025 Uiso 1 1 calc R U . . .
 C16 C 0.49535(17) 0.39712(12) 0.57408(14) 0.0174(4) Uani 1 1 d . . . . .
 H16 H 0.549301 0.441915 0.595424 0.021 Uiso 1 1 calc R U . . .
 C17 C 1.01260(18) 0.44642(12) 0.66315(14) 0.0187(4) Uani 1 1 d . . . . .
 C18 C 0.66962(19) 0.34134(14) 0.19669(14) 0.0218(4) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Fe1 O1 2.1442(14) . ?
 Fe1 O4 2.0641(13) . ?
 Fe1 O7 2.2359(13) . ?
 Fe1 N1 2.2366(15) . ?
 Fe1 N2 2.1233(15) . ?
 Fe1 N3 2.1404(16) . ?
 S1 O4 1.4655(13) . ?
 S1 O5 1.4329(16) . ?
 S1 O6 1.4297(15) . ?
 S1 C17 1.828(2) . ?
 S2 O7 1.4541(13) . ?
 S2 O8 1.4476(14) . ?
 S2 O9 1.4308(14) . ?
 S2 C18 1.830(2) . ?
 F1 C17 1.330(2) . ?
 F2 C17 1.327(2) . ?
 F3 C17 1.334(2) . ?
 F4 C18 1.335(2) . ?
 F5 C18 1.323(2) . ?
 F6 C18 1.328(2) . ?
 O1 H1 0.80(3) . ?
 O1 C1 1.431(2) . ?
 O2 C3 1.431(2) . ?
 O2 C4 1.410(2) . ?
 O3 C5 1.434(2) . ?
 O3 C6 1.409(2) . ?
 N1 C2 1.518(2) . ?
 N1 C4 1.488(2) . ?
 N1 C6 1.473(2) . ?
 N2 C7 1.345(2) . ?
 N2 C11 1.345(2) . ?
 N3 C12 1.341(2) . ?
 N3 C16 1.349(2) . ?
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C2 1.528(2) . ?
 C2 C3 1.525(3) . ?
 C2 C5 1.551(2) . ?
 C3 H3A 0.9700 . ?
 C3 H3B 0.9700 . ?
 C4 H4 0.9800 . ?
 C4 C7 1.528(2) . ?
 C5 H5A 0.9700 . ?
 C5 H5B 0.9700 . ?
 C6 H6 0.9800 . ?
 C6 C12 1.529(2) . ?
 C7 C8 1.386(3) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.388(3) . ?
 C9 H9 0.9300 . ?
 C9 C10 1.388(3) . ?
 C10 H10 0.9300 . ?
 C10 C11 1.381(3) . ?
 C11 H11 0.9300 . ?
 C12 C13 1.387(3) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.386(3) . ?
 C14 H14 0.9300 . ?
 C14 C15 1.385(3) . ?
 C15 H15 0.9300 . ?
 C15 C16 1.385(3) . ?
 C16 H16 0.9300 . ?

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
 O1 Fe1 O7 175.01(5) . . ?
 O1 Fe1 N1 75.24(5) . . ?
 O4 Fe1 O1 95.57(5) . . ?
 O4 Fe1 O7 84.31(5) . . ?
 O4 Fe1 N1 169.01(6) . . ?
 O4 Fe1 N2 108.56(6) . . ?
 O4 Fe1 N3 99.42(6) . . ?
 O7 Fe1 N1 105.37(5) . . ?
 N2 Fe1 O1 91.01(6) . . ?
 N2 Fe1 O7 84.31(5) . . ?
 N2 Fe1 N1 78.08(6) . . ?
 N2 Fe1 N3 149.21(6) . . ?
 N3 Fe1 O1 98.97(6) . . ?
 N3 Fe1 O7 85.95(5) . . ?
 N3 Fe1 N1 76.50(6) . . ?
 O4 S1 C17 101.66(8) . . ?
 O5 S1 O4 114.40(9) . . ?
 O5 S1 C17 104.44(9) . . ?
 O6 S1 O4 112.88(9) . . ?
 O6 S1 O5 117.36(10) . . ?
 O6 S1 C17 103.68(9) . . ?
 O7 S2 C18 103.02(8) . . ?
 O8 S2 O7 113.51(8) . . ?
 O8 S2 C18 102.48(9) . . ?
 O9 S2 O7 114.89(8) . . ?
 O9 S2 O8 115.94(9) . . ?
 O9 S2 C18 104.75(9) . . ?
 Fe1 O1 H1 139(2) . . ?
 C1 O1 Fe1 112.40(11) . . ?
 C1 O1 H1 108(2) . . ?
 C4 O2 C3 103.85(13) . . ?
 C6 O3 C5 105.38(13) . . ?
 S1 O4 Fe1 138.31(9) . . ?
 S2 O7 Fe1 139.79(8) . . ?
 C2 N1 Fe1 112.70(10) . . ?
 C4 N1 Fe1 111.58(11) . . ?
 C4 N1 C2 104.73(13) . . ?
 C6 N1 Fe1 110.22(10) . . ?
 C6 N1 C2 104.02(13) . . ?
 C6 N1 C4 113.30(14) . . ?
 C7 N2 Fe1 117.89(12) . . ?
 C11 N2 Fe1 123.60(13) . . ?
 C11 N2 C7 118.50(16) . . ?
 C12 N3 Fe1 116.50(12) . . ?
 C12 N3 C16 118.21(16) . . ?
 C16 N3 Fe1 125.03(13) . . ?
 O1 C1 H1A 110.0 . . ?
 O1 C1 H1B 110.0 . . ?
 O1 C1 C2 108.55(15) . . ?
 H1A C1 H1B 108.4 . . ?
 C2 C1 H1A 110.0 . . ?
 C2 C1 H1B 110.0 . . ?
 N1 C2 C1 110.50(14) . . ?
 N1 C2 C3 102.38(14) . . ?
 N1 C2 C5 103.77(14) . . ?
 C1 C2 C5 112.20(15) . . ?
 C3 C2 C1 113.94(16) . . ?
 C3 C2 C5 113.07(15) . . ?
 O2 C3 C2 104.00(15) . . ?
 O2 C3 H3A 111.0 . . ?
 O2 C3 H3B 111.0 . . ?
 C2 C3 H3A 111.0 . . ?
 C2 C3 H3B 111.0 . . ?
 H3A C3 H3B 109.0 . . ?
 O2 C4 N1 107.28(14) . . ?
 O2 C4 H4 108.9 . . ?
 O2 C4 C7 111.00(15) . . ?
 N1 C4 H4 108.9 . . ?
 N1 C4 C7 111.94(14) . . ?
 C7 C4 H4 108.9 . . ?
 O3 C5 C2 105.66(14) . . ?
 O3 C5 H5A 110.6 . . ?
 O3 C5 H5B 110.6 . . ?
 C2 C5 H5A 110.6 . . ?
 C2 C5 H5B 110.6 . . ?
 H5A C5 H5B 108.7 . . ?
 O3 C6 N1 107.16(14) . . ?
 O3 C6 H6 109.5 . . ?
 O3 C6 C12 111.22(14) . . ?
 N1 C6 H6 109.5 . . ?
 N1 C6 C12 109.92(14) . . ?
 C12 C6 H6 109.5 . . ?
 N2 C7 C4 118.09(16) . . ?
 N2 C7 C8 122.30(17) . . ?
 C8 C7 C4 119.43(17) . . ?
 C7 C8 H8 120.6 . . ?
 C7 C8 C9 118.85(18) . . ?
 C9 C8 H8 120.6 . . ?
 C8 C9 H9 120.5 . . ?
 C10 C9 C8 118.95(18) . . ?
 C10 C9 H9 120.5 . . ?
 C9 C10 H10 120.6 . . ?
 C11 C10 C9 118.84(18) . . ?
 C11 C10 H10 120.6 . . ?
 N2 C11 C10 122.55(18) . . ?
 N2 C11 H11 118.7 . . ?
 C10 C11 H11 118.7 . . ?
 N3 C12 C6 118.28(15) . . ?
 N3 C12 C13 122.51(17) . . ?
 C13 C12 C6 119.14(16) . . ?
 C12 C13 H13 120.6 . . ?
 C14 C13 C12 118.75(18) . . ?
 C14 C13 H13 120.6 . . ?
 C13 C14 H14 120.3 . . ?
 C15 C14 C13 119.33(18) . . ?
 C15 C14 H14 120.3 . . ?
 C14 C15 H15 120.8 . . ?
 C16 C15 C14 118.47(18) . . ?
 C16 C15 H15 120.8 . . ?
 N3 C16 C15 122.72(18) . . ?
 N3 C16 H16 118.6 . . ?
 C15 C16 H16 118.6 . . ?
 F1 C17 S1 110.29(13) . . ?
 F1 C17 F3 108.21(16) . . ?
 F2 C17 S1 111.93(13) . . ?
 F2 C17 F1 107.89(16) . . ?
 F2 C17 F3 107.60(16) . . ?
 F3 C17 S1 110.79(13) . . ?
 F4 C18 S2 110.08(14) . . ?
 F5 C18 S2 111.39(14) . . ?
 F5 C18 F4 108.42(16) . . ?
 F5 C18 F6 108.43(17) . . ?
 F6 C18 S2 110.55(13) . . ?
 F6 C18 F4 107.87(17) . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O1 H1 O8 0.80(3) 1.94(3) 2.719(2) 165(3) 4_666 yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Fe1 O1 C1 C2 51.43(17) . . . . ?
 Fe1 N1 C2 C1 9.60(17) . . . . ?
 Fe1 N1 C2 C3 -112.12(13) . . . . ?
 Fe1 N1 C2 C5 130.06(12) . . . . ?
 Fe1 N1 C4 O2 138.62(11) . . . . ?
 Fe1 N1 C4 C7 16.61(17) . . . . ?
 Fe1 N1 C6 O3 -151.71(11) . . . . ?
 Fe1 N1 C6 C12 -30.73(16) . . . . ?
 Fe1 N2 C7 C4 7.0(2) . . . . ?
 Fe1 N2 C7 C8 -177.90(14) . . . . ?
 Fe1 N2 C11 C10 178.31(14) . . . . ?
 Fe1 N3 C12 C6 2.2(2) . . . . ?
 Fe1 N3 C12 C13 -174.72(14) . . . . ?
 Fe1 N3 C16 C15 172.89(14) . . . . ?
 O1 C1 C2 N1 -38.2(2) . . . . ?
 O1 C1 C2 C3 76.40(19) . . . . ?
 O1 C1 C2 C5 -153.50(15) . . . . ?
 O2 C4 C7 N2 -135.91(16) . . . . ?
 O2 C4 C7 C8 48.8(2) . . . . ?
 O3 C6 C12 N3 138.57(16) . . . . ?
 O3 C6 C12 C13 -44.4(2) . . . . ?
 O4 S1 C17 F1 -179.47(13) . . . . ?
 O4 S1 C17 F2 60.41(15) . . . . ?
 O4 S1 C17 F3 -59.69(15) . . . . ?
 O5 S1 O4 Fe1 -22.35(17) . . . . ?
 O5 S1 C17 F1 -60.22(15) . . . . ?
 O5 S1 C17 F2 179.66(13) . . . . ?
 O5 S1 C17 F3 59.56(15) . . . . ?
 O6 S1 O4 Fe1 -160.01(12) . . . . ?
 O6 S1 C17 F1 63.22(15) . . . . ?
 O6 S1 C17 F2 -56.90(16) . . . . ?
 O6 S1 C17 F3 -177.00(14) . . . . ?
 O7 S2 C18 F4 177.03(14) . . . . ?
 O7 S2 C18 F5 -62.67(16) . . . . ?
 O7 S2 C18 F6 57.95(15) . . . . ?
 O8 S2 O7 Fe1 0.47(16) . . . . ?
 O8 S2 C18 F4 58.97(16) . . . . ?
 O8 S2 C18 F5 179.27(14) . . . . ?
 O8 S2 C18 F6 -60.11(15) . . . . ?
 O9 S2 O7 Fe1 137.16(12) . . . . ?
 O9 S2 C18 F4 -62.47(16) . . . . ?
 O9 S2 C18 F5 57.83(16) . . . . ?
 O9 S2 C18 F6 178.45(13) . . . . ?
 N1 C2 C3 O2 -31.63(17) . . . . ?
 N1 C2 C5 O3 11.82(17) . . . . ?
 N1 C4 C7 N2 -16.1(2) . . . . ?
 N1 C4 C7 C8 168.66(16) . . . . ?
 N1 C6 C12 N3 20.1(2) . . . . ?
 N1 C6 C12 C13 -162.95(16) . . . . ?
 N2 C7 C8 C9 -0.4(3) . . . . ?
 N3 C12 C13 C14 1.4(3) . . . . ?
 C1 C2 C3 O2 -150.96(15) . . . . ?
 C1 C2 C5 O3 131.13(15) . . . . ?
 C2 N1 C4 O2 16.41(18) . . . . ?
 C2 N1 C4 C7 -105.59(16) . . . . ?
 C2 N1 C6 O3 -30.67(17) . . . . ?
 C2 N1 C6 C12 90.32(16) . . . . ?
 C3 O2 C4 N1 -37.29(18) . . . . ?
 C3 O2 C4 C7 85.30(17) . . . . ?
 C3 C2 C5 O3 -98.32(17) . . . . ?
 C4 O2 C3 C2 42.90(17) . . . . ?
 C4 N1 C2 C1 131.07(15) . . . . ?
 C4 N1 C2 C3 9.36(17) . . . . ?
 C4 N1 C2 C5 -108.47(15) . . . . ?
 C4 N1 C6 O3 82.46(17) . . . . ?
 C4 N1 C6 C12 -156.55(14) . . . . ?
 C4 C7 C8 C9 174.69(18) . . . . ?
 C5 O3 C6 N1 39.32(17) . . . . ?
 C5 O3 C6 C12 -80.84(17) . . . . ?
 C5 C2 C3 O2 79.37(18) . . . . ?
 C6 O3 C5 C2 -31.06(17) . . . . ?
 C6 N1 C2 C1 -109.77(16) . . . . ?
 C6 N1 C2 C3 128.51(15) . . . . ?
 C6 N1 C2 C5 10.69(17) . . . . ?
 C6 N1 C4 O2 -96.29(17) . . . . ?
 C6 N1 C4 C7 141.71(15) . . . . ?
 C6 C12 C13 C14 -175.46(17) . . . . ?
 C7 N2 C11 C10 -0.6(3) . . . . ?
 C7 C8 C9 C10 -0.8(3) . . . . ?
 C8 C9 C10 C11 1.2(3) . . . . ?
 C9 C10 C11 N2 -0.6(3) . . . . ?
 C11 N2 C7 C4 -174.07(16) . . . . ?
 C11 N2 C7 C8 1.1(3) . . . . ?
 C12 N3 C16 C15 -1.0(3) . . . . ?
 C12 C13 C14 C15 -1.2(3) . . . . ?
 C13 C14 C15 C16 0.0(3) . . . . ?
 C14 C15 C16 N3 1.2(3) . . . . ?
 C16 N3 C12 C6 176.59(16) . . . . ?
 C16 N3 C12 C13 -0.3(3) . . . . ?
 C17 S1 O4 Fe1 89.56(14) . . . . ?
 C18 S2 O7 Fe1 -109.55(13) . . . . ?


_olex2_submission_original_sample_id  jonon95
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.424
_oxdiff_exptl_absorpt_empirical_full_min  0.822
#===end
data_B
_audit_creation_date               2020-11-19
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

#CrysAlisPro, version 171.40.84a
Rigaku Oxford Diffraction (2020). CrysAlisPro Software system,
version 171.40.84a. Rigaku Corporation, Oxford, UK.

#SHELXT-2018/2
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3--8.

#SHELXL-2018/3
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3--8.
;
_publ_contact_author_name        'William D. Jones'
_publ_contact_author_address     
;
 'Department of Chemistry, University of Rochester, Rochester, New York 14627'
;
_publ_contact_author_email       'jones@chem.rochester.edu'
_publ_requested_journal          'J. Am. Chem. Soc.'
_publ_section_title            
;
Iron-Based Dehydration Catalyst for Selective Formation of Styrene
;

loop_
_publ_author_name                
 'Olaf Nachtigall'
 'Andrew I. VanderWeide'
 'William W. Brennessel'
 'William D. Jones'

_publ_author_address             
;
 Department of Chemistry, University of Rochester, Rochester, NY  14627 USA
;

_chemical_name_common              jonon94
_chemical_name_systematic          '[(FOX)Fe(CyOH)(OTf)][OTf-CyOH]'
_chemical_formula_moiety           'C23 H29 F3 Fe N3 O7 S, C F3 O3 S, C6 H12 O'
_chemical_formula_sum              'C30 H41 F6 Fe N3 O11 S2'
_chemical_formula_weight           853.63
_chemical_melting_point            ?
_chemical_oxdiff_formula           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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'
 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe' 'Fe' -1.1336 3.1974
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     10.0940(2)
_cell_length_b                     13.5688(3)
_cell_length_c                     14.2285(2)
_cell_angle_alpha                  77.548(2)
_cell_angle_beta                   80.246(2)
_cell_angle_gamma                  80.970(2)
_cell_volume                       1860.70(6)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      29439
_cell_measurement_temperature      100.00(13)
_cell_measurement_theta_max        77.2340
_cell_measurement_theta_min        3.2270
_shelx_estimated_absorpt_T_max     0.923
_shelx_estimated_absorpt_T_min     0.377
_exptl_absorpt_coefficient_mu      5.107
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.58008
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'light yellow'
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.524
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               884
_exptl_crystal_size_max            0.237
_exptl_crystal_size_mid            0.135
_exptl_crystal_size_min            0.0159
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0710
_diffrn_reflns_av_unetI/netI       0.0384
_diffrn_reflns_Laue_measured_fraction_full  0.998
_diffrn_reflns_Laue_measured_fraction_max  0.973
_diffrn_reflns_limit_h_max         12
_diffrn_reflns_limit_h_min         -12
_diffrn_reflns_limit_k_max         16
_diffrn_reflns_limit_k_min         -17
_diffrn_reflns_limit_l_max         16
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              46235
_diffrn_reflns_point_group_measured_fraction_full  0.998
_diffrn_reflns_point_group_measured_fraction_max  0.973
_diffrn_reflns_theta_full          74.504
_diffrn_reflns_theta_max           79.127
_diffrn_reflns_theta_min           3.213
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        100.00(13)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  0.998
_diffrn_measured_fraction_theta_max  0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -21.00  75.00   0.50    0.17    --   49.75 -87.00-111.00  192
  2  ω     34.00 131.00   0.50    0.68    --  105.75 -87.00-111.00  194
  3  ω     98.00 164.00   0.50    0.68    --  105.75  15.00 -60.00  132
  4  ω     98.00 178.00   0.50    0.68    --  105.75  87.00   6.00  160
  5  ω     98.00 164.00   0.50    0.68    --  105.75  15.00   0.00  132
  6  ω     98.00 178.00   0.50    0.68    --  105.75  30.00  30.00  160
  7  ω     98.00 164.00   0.50    0.68    --  105.75  15.00  90.00  132
  8  ω     92.00 178.00   0.50    0.68    --  105.75  61.00 -30.00  172
  9  ω     98.00 178.00   0.50    0.68    --  105.75  30.00-180.00  160
 10  ω     92.00 178.00   0.50    0.68    --  105.75 125.00-120.00  172
 11  ω     92.00 178.00   0.50    0.68    --  105.75  61.00  60.00  172
 12  ω     83.00 178.00   0.50    0.68    --  105.75  81.00 -84.84  190
 13  ω     92.00 178.00   0.50    0.68    --  105.75 125.00-150.00  172
 14  ω     34.00  87.00   0.50    0.68    --  105.75 -61.00-120.00  106
 15  ω     34.00 113.00   0.50    0.68    --  105.75-118.00-156.77  158
 16  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00   0.00  150
 17  ω     34.00 116.00   0.50    0.68    --  105.75-125.00 150.00  164
 18  ω     34.00  87.00   0.50    0.68    --  105.75 -61.00 150.00  106
 19  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00  60.00  150
 20  ω     34.00 111.00   0.50    0.68    --  105.75-108.00 -28.82  154
 21  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00-180.00  150
 22  ω     34.00 127.00   0.50    0.68    --  105.75 -77.00-150.00  186
 23  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00-120.00  150
 24  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00-150.00  150
 25  ω     34.00  87.00   0.50    0.68    --  105.75 -61.00   0.00  106
 26  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00  30.00  150
 27  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00 -30.00  150
 28  ω     34.00  87.00   0.50    0.68    --  105.75 -61.00 -60.00  106
 29  ω     34.00  87.00   0.50    0.68    --  105.75 -61.00  30.00  106
 30  ω     34.00 116.00   0.50    0.68    --  105.75-125.00  90.00  164
 31  ω     34.00 109.00   0.50    0.68    --  105.75 -94.00 150.00  150
 32  ω    -23.00   5.00   0.50    0.17    --   49.75 -19.00 120.00   56
 33  ω    -23.00   5.00   0.50    0.17    --   49.75 -19.00   0.00   56
 34  ω    -23.00   5.00   0.50    0.17    --   49.75 -19.00 -60.00   56
 35  ω    -23.00   5.00   0.50    0.17    --   49.75 -19.00 -90.00   56
 36  ω    -23.00   5.00   0.50    0.17    --   49.75 -19.00 -30.00   56
 37  ω     29.00  90.00   0.50    0.17    --   49.75  77.00 -30.00  122
 38  ω     29.00 121.00   0.50    0.17    --   49.75  77.00-120.00  184
 39  ω    -30.00  22.00   0.50    0.17    --  -49.75  38.00 -90.00  104
 40  ω    -42.00 -12.00   0.50    0.68    --  -84.25  45.00-150.00   60
 41  ω    -75.00  22.00   0.50    0.17    --  -49.75  87.00   6.00  194
 42  ω    -42.00 -12.00   0.50    0.68    --  -84.25  45.00   0.00   60
 43  ω   -109.00 -12.00   0.50    0.68    --  -84.25  87.00   6.00  194
 44  ω   -121.00 -37.00   0.50    0.17    --  -49.75 -57.00 120.00  168
 45  ω   -121.00 -70.00   0.50    0.17    --  -49.75-125.00   0.00  102
 46  ω   -121.00 -70.00   0.50    0.17    --  -49.75-125.00  30.00  102
 47  ω   -121.00 -70.00   0.50    0.17    --  -49.75-125.00 120.00  102
 48  ω   -156.00 -76.00   0.50    0.68    --  -84.25 -87.00-111.00  160
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0741155000
_diffrn_orient_matrix_UB_12        -0.0886981000
_diffrn_orient_matrix_UB_13        0.0609790000
_diffrn_orient_matrix_UB_21        -0.0893366000
_diffrn_orient_matrix_UB_22        0.0106005000
_diffrn_orient_matrix_UB_23        -0.0802029000
_diffrn_orient_matrix_UB_31        0.1043497000
_diffrn_orient_matrix_UB_32        -0.0758595000
_diffrn_orient_matrix_UB_33        -0.0489038000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Cu K\a'
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  7318
_reflns_number_total               7836
_reflns_odcompleteness_completeness  99.86
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max           0.528
_refine_diff_density_min           -0.613
_refine_diff_density_rms           0.088
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.127
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       490
_refine_ls_number_reflns           7836
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0538
_refine_ls_R_factor_gt             0.0508
_refine_ls_restrained_S_all        1.127
_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)+(0.0865P)²+1.2450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1407
_refine_ls_wR_factor_ref           0.1472
_refine_special_details            ?
_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), C6(H6), C18(H18), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B),
  C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap
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
 Fe1 Fe 0.39222(3) 0.29962(3) 0.30484(3) 0.01909(12) Uani 1 1 d . . . . .
 S1 S 0.16461(6) 0.22288(4) 0.51116(4) 0.02345(14) Uani 1 1 d . . . . .
 F1 F 0.1318(2) 0.19948(16) 0.69963(12) 0.0494(5) Uani 1 1 d . . . . .
 F2 F 0.32007(19) 0.12177(14) 0.63905(13) 0.0418(4) Uani 1 1 d . . . . .
 F3 F 0.2952(2) 0.28447(16) 0.62690(16) 0.0554(5) Uani 1 1 d . . . . .
 O1 O 0.51174(19) 0.37572(13) 0.18164(13) 0.0252(4) Uani 1 1 d . . . . .
 H1 H 0.571(4) 0.358(3) 0.130(3) 0.052(11) Uiso 1 1 d . . . . .
 O2 O 0.62997(17) 0.47880(13) 0.39663(13) 0.0231(3) Uani 1 1 d . . . . .
 O3 O 0.33710(17) 0.59044(12) 0.38045(13) 0.0234(4) Uani 1 1 d . . . . .
 O4 O 0.2865(2) 0.22924(17) 0.44069(15) 0.0368(5) Uani 1 1 d . . . . .
 O5 O 0.0723(2) 0.31475(16) 0.50674(16) 0.0398(5) Uani 1 1 d . . . . .
 O6 O 0.1070(2) 0.13107(15) 0.52026(16) 0.0359(4) Uani 1 1 d . . . . .
 O7 O 0.37115(19) 0.18770(13) 0.23421(15) 0.0279(4) Uani 1 1 d . . . . .
 H7 H 0.352(6) 0.208(4) 0.169(4) 0.090(17) Uiso 1 1 d . . . . .
 N1 N 0.4382(2) 0.43285(15) 0.35371(14) 0.0195(4) Uani 1 1 d . . . . .
 N2 N 0.5657(2) 0.23736(15) 0.37471(15) 0.0211(4) Uani 1 1 d . . . . .
 N3 N 0.2156(2) 0.40796(16) 0.28271(16) 0.0233(4) Uani 1 1 d . . . . .
 C1 C 0.4929(3) 0.48450(18) 0.17199(18) 0.0247(5) Uani 1 1 d . . . . .
 H1A H 0.405487 0.512466 0.151522 0.030 Uiso 1 1 calc R U . . .
 H1B H 0.562880 0.514079 0.123516 0.030 Uiso 1 1 calc R U . . .
 C2 C 0.5002(2) 0.50929(17) 0.27086(17) 0.0214(5) Uani 1 1 d . . . . .
 C3 C 0.6450(2) 0.50052(18) 0.29241(18) 0.0229(5) Uani 1 1 d . . . . .
 H3A H 0.702345 0.445923 0.265645 0.027 Uiso 1 1 calc R U . . .
 H3B H 0.683442 0.563650 0.266070 0.027 Uiso 1 1 calc R U . . .
 C4 C 0.5399(2) 0.40360(17) 0.42243(17) 0.0202(4) Uani 1 1 d . . . . .
 H4 H 0.494216 0.403013 0.489012 0.024 Uiso 1 1 calc R U . . .
 C5 C 0.4176(3) 0.61234(18) 0.28690(18) 0.0246(5) Uani 1 1 d . . . . .
 H5A H 0.477597 0.661883 0.285993 0.029 Uiso 1 1 calc R U . . .
 H5B H 0.360180 0.638939 0.236623 0.029 Uiso 1 1 calc R U . . .
 C6 C 0.3102(2) 0.48897(17) 0.39091(17) 0.0210(5) Uani 1 1 d . . . . .
 H6 H 0.282304 0.460068 0.459439 0.025 Uiso 1 1 calc R U . . .
 C7 C 0.6194(2) 0.29918(18) 0.41558(17) 0.0202(4) Uani 1 1 d . . . . .
 C8 C 0.7417(3) 0.2702(2) 0.45265(19) 0.0258(5) Uani 1 1 d . . . . .
 H8 H 0.778314 0.315094 0.479024 0.031 Uiso 1 1 calc R U . . .
 C9 C 0.8083(3) 0.1729(2) 0.44954(19) 0.0273(5) Uani 1 1 d . . . . .
 H9 H 0.891026 0.151954 0.472693 0.033 Uiso 1 1 calc R U . . .
 C10 C 0.7488(3) 0.1073(2) 0.4111(2) 0.0290(5) Uani 1 1 d . . . . .
 H10 H 0.788979 0.040824 0.410901 0.035 Uiso 1 1 calc R U . . .
 C11 C 0.6296(3) 0.14273(19) 0.3736(2) 0.0268(5) Uani 1 1 d . . . . .
 H11 H 0.591484 0.099431 0.346217 0.032 Uiso 1 1 calc R U . . .
 C12 C 0.2003(2) 0.48551(18) 0.32991(17) 0.0220(5) Uani 1 1 d . . . . .
 C13 C 0.0922(3) 0.5627(2) 0.3219(2) 0.0297(5) Uani 1 1 d . . . . .
 H13 H 0.082308 0.614604 0.356893 0.036 Uiso 1 1 calc R U . . .
 C14 C -0.0009(3) 0.5609(2) 0.2606(2) 0.0334(6) Uani 1 1 d . . . . .
 H14 H -0.073223 0.612297 0.253293 0.040 Uiso 1 1 calc R U . . .
 C15 C 0.0155(3) 0.4818(2) 0.2107(2) 0.0325(6) Uani 1 1 d . . . . .
 H15 H -0.044890 0.479497 0.168848 0.039 Uiso 1 1 calc R U . . .
 C16 C 0.1244(3) 0.4057(2) 0.2246(2) 0.0279(5) Uani 1 1 d . . . . .
 H16 H 0.134302 0.351492 0.192612 0.033 Uiso 1 1 calc R U . . .
 C17 C 0.2314(3) 0.2063(2) 0.6249(2) 0.0322(6) Uani 1 1 d . . . . .
 C18 C 0.3165(3) 0.09208(18) 0.27741(19) 0.0243(5) Uani 1 1 d . . . . .
 H18 H 0.327137 0.075695 0.346455 0.029 Uiso 1 1 calc R U . . .
 C19 C 0.3966(3) 0.0077(2) 0.2297(2) 0.0306(6) Uani 1 1 d . . . . .
 H19A H 0.491113 0.001557 0.238165 0.037 Uiso 1 1 calc R U . . .
 H19B H 0.391229 0.023935 0.160494 0.037 Uiso 1 1 calc R U . . .
 C20 C 0.3411(4) -0.0936(2) 0.2745(3) 0.0435(8) Uani 1 1 d . . . . .
 H20A H 0.389198 -0.145839 0.239940 0.052 Uiso 1 1 calc R U . . .
 H20B H 0.356542 -0.113734 0.341770 0.052 Uiso 1 1 calc R U . . .
 C21 C 0.1906(4) -0.0852(3) 0.2696(3) 0.0482(8) Uani 1 1 d . . . . .
 H21A H 0.157063 -0.148527 0.303119 0.058 Uiso 1 1 calc R U . . .
 H21B H 0.176307 -0.074122 0.202159 0.058 Uiso 1 1 calc R U . . .
 C22 C 0.1112(3) 0.0020(2) 0.3155(2) 0.0393(7) Uani 1 1 d . . . . .
 H22A H 0.116141 -0.013133 0.384760 0.047 Uiso 1 1 calc R U . . .
 H22B H 0.016670 0.008324 0.306988 0.047 Uiso 1 1 calc R U . . .
 C23 C 0.1669(3) 0.1024(2) 0.2699(2) 0.0288(5) Uani 1 1 d . . . . .
 H23A H 0.153475 0.121394 0.202148 0.035 Uiso 1 1 calc R U . . .
 H23B H 0.118453 0.155620 0.303102 0.035 Uiso 1 1 calc R U . . .
 S2 S 0.31500(7) 0.27827(5) -0.04691(5) 0.03028(16) Uani 1 1 d . . . . .
 F4 F 0.3303(2) 0.15701(19) -0.16857(16) 0.0612(6) Uani 1 1 d . . . . .
 F5 F 0.1746(3) 0.1331(2) -0.0474(3) 0.0834(9) Uani 1 1 d . . . . .
 F6 F 0.3837(3) 0.08226(15) -0.03033(16) 0.0559(5) Uani 1 1 d . . . . .
 O8 O 0.2851(3) 0.26200(17) 0.05728(15) 0.0433(5) Uani 1 1 d . . . . .
 O9 O 0.4543(2) 0.29068(19) -0.08515(17) 0.0434(5) Uani 1 1 d . . . . .
 O10 O 0.2183(3) 0.34818(19) -0.09771(17) 0.0471(6) Uani 1 1 d . . . . .
 C24 C 0.2999(3) 0.1550(3) -0.0741(2) 0.0396(7) Uani 1 1 d . . . . .
 O11 O 0.6354(2) 0.33756(18) 0.01715(15) 0.0377(5) Uani 1 1 d . . . . .
 H11A H 0.566(4) 0.319(3) -0.009(3) 0.048(11) Uiso 1 1 d . . . . .
 C25 C 0.7781(3) 0.3165(3) -0.0193(2) 0.0450(7) Uani 1 1 d . . . . .
 H25 H 0.800070 0.368044 -0.077460 0.054 Uiso 1 1 calc R U . . .
 C26 C 0.8591(4) 0.3261(4) 0.0568(3) 0.0606(11) Uani 1 1 d . . . . .
 H26A H 0.953814 0.324321 0.028895 0.073 Uiso 1 1 calc R U . . .
 H26B H 0.830137 0.391741 0.075257 0.073 Uiso 1 1 calc R U . . .
 C27 C 0.8461(4) 0.2462(5) 0.1442(3) 0.0729(14) Uani 1 1 d . . . . .
 H27A H 0.754493 0.254566 0.178243 0.087 Uiso 1 1 calc R U . . .
 H27B H 0.907539 0.253316 0.187184 0.087 Uiso 1 1 calc R U . . .
 C28 C 0.8773(5) 0.1408(5) 0.1202(4) 0.0859(18) Uani 1 1 d . . . . .
 H28A H 0.857694 0.090385 0.178718 0.103 Uiso 1 1 calc R U . . .
 H28B H 0.972803 0.128007 0.095686 0.103 Uiso 1 1 calc R U . . .
 C29 C 0.7909(7) 0.1313(4) 0.0427(6) 0.103(2) Uani 1 1 d . . . . .
 H29A H 0.817478 0.065638 0.023961 0.124 Uiso 1 1 calc R U . . .
 H29B H 0.696072 0.135214 0.070524 0.124 Uiso 1 1 calc R U . . .
 C30 C 0.8092(5) 0.2150(4) -0.0467(3) 0.0682(13) Uani 1 1 d . . . . .
 H30A H 0.901868 0.206582 -0.078827 0.082 Uiso 1 1 calc R U . . .
 H30B H 0.749669 0.210120 -0.091827 0.082 Uiso 1 1 calc R U . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Fe1 O1 2.1186(18) . ?
 Fe1 O4 2.1478(19) . ?
 Fe1 O7 2.0478(18) . ?
 Fe1 N1 2.2096(19) . ?
 Fe1 N2 2.129(2) . ?
 Fe1 N3 2.146(2) . ?
 S1 O4 1.4504(19) . ?
 S1 O5 1.431(2) . ?
 S1 O6 1.428(2) . ?
 S1 C17 1.814(3) . ?
 F1 C17 1.331(3) . ?
 F2 C17 1.340(3) . ?
 F3 C17 1.332(3) . ?
 O1 H1 0.92(4) . ?
 O1 C1 1.438(3) . ?
 O2 C3 1.435(3) . ?
 O2 C4 1.421(3) . ?
 O3 C5 1.435(3) . ?
 O3 C6 1.417(3) . ?
 O7 H7 0.95(6) . ?
 O7 C18 1.460(3) . ?
 N1 C2 1.511(3) . ?
 N1 C4 1.487(3) . ?
 N1 C6 1.471(3) . ?
 N2 C7 1.340(3) . ?
 N2 C11 1.345(3) . ?
 N3 C12 1.342(3) . ?
 N3 C16 1.345(3) . ?
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C2 1.531(3) . ?
 C2 C3 1.526(3) . ?
 C2 C5 1.552(3) . ?
 C3 H3A 0.9700 . ?
 C3 H3B 0.9700 . ?
 C4 H4 0.9800 . ?
 C4 C7 1.528(3) . ?
 C5 H5A 0.9700 . ?
 C5 H5B 0.9700 . ?
 C6 H6 0.9800 . ?
 C6 C12 1.531(3) . ?
 C7 C8 1.392(3) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.390(4) . ?
 C9 H9 0.9300 . ?
 C9 C10 1.392(4) . ?
 C10 H10 0.9300 . ?
 C10 C11 1.375(4) . ?
 C11 H11 0.9300 . ?
 C12 C13 1.390(3) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.392(4) . ?
 C14 H14 0.9300 . ?
 C14 C15 1.385(4) . ?
 C15 H15 0.9300 . ?
 C15 C16 1.394(4) . ?
 C16 H16 0.9300 . ?
 C18 H18 0.9800 . ?
 C18 C19 1.512(3) . ?
 C18 C23 1.514(4) . ?
 C19 H19A 0.9700 . ?
 C19 H19B 0.9700 . ?
 C19 C20 1.534(4) . ?
 C20 H20A 0.9700 . ?
 C20 H20B 0.9700 . ?
 C20 C21 1.518(5) . ?
 C21 H21A 0.9700 . ?
 C21 H21B 0.9700 . ?
 C21 C22 1.526(4) . ?
 C22 H22A 0.9700 . ?
 C22 H22B 0.9700 . ?
 C22 C23 1.527(4) . ?
 C23 H23A 0.9700 . ?
 C23 H23B 0.9700 . ?
 S2 O8 1.437(2) . ?
 S2 O9 1.441(2) . ?
 S2 O10 1.424(2) . ?
 S2 C24 1.831(3) . ?
 F4 C24 1.323(4) . ?
 F5 C24 1.319(4) . ?
 F6 C24 1.315(4) . ?
 O11 H11A 0.93(4) . ?
 O11 C25 1.452(4) . ?
 C25 H25 0.9800 . ?
 C25 C26 1.500(5) . ?
 C25 C30 1.483(5) . ?
 C26 H26A 0.9700 . ?
 C26 H26B 0.9700 . ?
 C26 C27 1.465(7) . ?
 C27 H27A 0.9700 . ?
 C27 H27B 0.9700 . ?
 C27 C28 1.515(8) . ?
 C28 H28A 0.9700 . ?
 C28 H28B 0.9700 . ?
 C28 C29 1.555(9) . ?
 C29 H29A 0.9700 . ?
 C29 H29B 0.9700 . ?
 C29 C30 1.518(8) . ?
 C30 H30A 0.9700 . ?
 C30 H30B 0.9700 . ?

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
 O1 Fe1 O4 172.66(8) . . ?
 O1 Fe1 N1 76.39(7) . . ?
 O1 Fe1 N2 91.97(8) . . ?
 O1 Fe1 N3 93.17(8) . . ?
 O4 Fe1 N1 97.44(8) . . ?
 O7 Fe1 O1 92.34(7) . . ?
 O7 Fe1 O4 93.81(8) . . ?
 O7 Fe1 N1 168.73(8) . . ?
 O7 Fe1 N2 102.64(8) . . ?
 O7 Fe1 N3 103.98(8) . . ?
 N2 Fe1 O4 82.78(8) . . ?
 N2 Fe1 N1 78.25(8) . . ?
 N2 Fe1 N3 152.63(8) . . ?
 N3 Fe1 O4 89.23(8) . . ?
 N3 Fe1 N1 76.90(8) . . ?
 O4 S1 C17 102.00(13) . . ?
 O5 S1 O4 114.87(13) . . ?
 O5 S1 C17 104.97(13) . . ?
 O6 S1 O4 112.82(13) . . ?
 O6 S1 O5 116.55(14) . . ?
 O6 S1 C17 103.36(13) . . ?
 Fe1 O1 H1 137(3) . . ?
 C1 O1 Fe1 113.68(14) . . ?
 C1 O1 H1 110(3) . . ?
 C4 O2 C3 103.12(17) . . ?
 C6 O3 C5 105.11(17) . . ?
 S1 O4 Fe1 150.30(14) . . ?
 Fe1 O7 H7 117(3) . . ?
 C18 O7 Fe1 126.94(15) . . ?
 C18 O7 H7 109(3) . . ?
 C2 N1 Fe1 112.46(13) . . ?
 C4 N1 Fe1 111.82(13) . . ?
 C4 N1 C2 104.85(17) . . ?
 C6 N1 Fe1 108.70(14) . . ?
 C6 N1 C2 104.04(17) . . ?
 C6 N1 C4 114.73(18) . . ?
 C7 N2 Fe1 117.43(16) . . ?
 C7 N2 C11 118.6(2) . . ?
 C11 N2 Fe1 123.74(17) . . ?
 C12 N3 Fe1 115.24(16) . . ?
 C12 N3 C16 118.8(2) . . ?
 C16 N3 Fe1 125.89(17) . . ?
 O1 C1 H1A 110.1 . . ?
 O1 C1 H1B 110.1 . . ?
 O1 C1 C2 108.18(19) . . ?
 H1A C1 H1B 108.4 . . ?
 C2 C1 H1A 110.1 . . ?
 C2 C1 H1B 110.1 . . ?
 N1 C2 C1 111.68(18) . . ?
 N1 C2 C3 102.40(19) . . ?
 N1 C2 C5 103.50(18) . . ?
 C1 C2 C5 113.5(2) . . ?
 C3 C2 C1 113.0(2) . . ?
 C3 C2 C5 111.81(19) . . ?
 O2 C3 C2 103.32(18) . . ?
 O2 C3 H3A 111.1 . . ?
 O2 C3 H3B 111.1 . . ?
 C2 C3 H3A 111.1 . . ?
 C2 C3 H3B 111.1 . . ?
 H3A C3 H3B 109.1 . . ?
 O2 C4 N1 106.78(18) . . ?
 O2 C4 H4 109.6 . . ?
 O2 C4 C7 109.62(18) . . ?
 N1 C4 H4 109.6 . . ?
 N1 C4 C7 111.61(18) . . ?
 C7 C4 H4 109.6 . . ?
 O3 C5 C2 105.46(19) . . ?
 O3 C5 H5A 110.6 . . ?
 O3 C5 H5B 110.6 . . ?
 C2 C5 H5A 110.6 . . ?
 C2 C5 H5B 110.6 . . ?
 H5A C5 H5B 108.8 . . ?
 O3 C6 N1 105.61(18) . . ?
 O3 C6 H6 110.4 . . ?
 O3 C6 C12 110.13(19) . . ?
 N1 C6 H6 110.4 . . ?
 N1 C6 C12 109.67(18) . . ?
 C12 C6 H6 110.4 . . ?
 N2 C7 C4 117.7(2) . . ?
 N2 C7 C8 122.1(2) . . ?
 C8 C7 C4 120.2(2) . . ?
 C7 C8 H8 120.6 . . ?
 C9 C8 C7 118.8(2) . . ?
 C9 C8 H8 120.6 . . ?
 C8 C9 H9 120.6 . . ?
 C8 C9 C10 118.8(2) . . ?
 C10 C9 H9 120.6 . . ?
 C9 C10 H10 120.6 . . ?
 C11 C10 C9 118.8(2) . . ?
 C11 C10 H10 120.6 . . ?
 N2 C11 C10 122.8(2) . . ?
 N2 C11 H11 118.6 . . ?
 C10 C11 H11 118.6 . . ?
 N3 C12 C6 117.5(2) . . ?
 N3 C12 C13 122.2(2) . . ?
 C13 C12 C6 120.2(2) . . ?
 C12 C13 H13 120.6 . . ?
 C12 C13 C14 118.8(2) . . ?
 C14 C13 H13 120.6 . . ?
 C13 C14 H14 120.4 . . ?
 C15 C14 C13 119.3(2) . . ?
 C15 C14 H14 120.4 . . ?
 C14 C15 H15 120.7 . . ?
 C14 C15 C16 118.6(3) . . ?
 C16 C15 H15 120.7 . . ?
 N3 C16 C15 122.3(2) . . ?
 N3 C16 H16 118.8 . . ?
 C15 C16 H16 118.8 . . ?
 F1 C17 S1 110.7(2) . . ?
 F1 C17 F2 108.0(2) . . ?
 F1 C17 F3 107.7(2) . . ?
 F2 C17 S1 111.52(18) . . ?
 F3 C17 S1 111.3(2) . . ?
 F3 C17 F2 107.5(2) . . ?
 O7 C18 H18 108.1 . . ?
 O7 C18 C19 109.7(2) . . ?
 O7 C18 C23 110.7(2) . . ?
 C19 C18 H18 108.1 . . ?
 C19 C18 C23 112.0(2) . . ?
 C23 C18 H18 108.1 . . ?
 C18 C19 H19A 109.6 . . ?
 C18 C19 H19B 109.6 . . ?
 C18 C19 C20 110.4(2) . . ?
 H19A C19 H19B 108.1 . . ?
 C20 C19 H19A 109.6 . . ?
 C20 C19 H19B 109.6 . . ?
 C19 C20 H20A 109.4 . . ?
 C19 C20 H20B 109.4 . . ?
 H20A C20 H20B 108.0 . . ?
 C21 C20 C19 111.3(3) . . ?
 C21 C20 H20A 109.4 . . ?
 C21 C20 H20B 109.4 . . ?
 C20 C21 H21A 109.3 . . ?
 C20 C21 H21B 109.3 . . ?
 C20 C21 C22 111.5(3) . . ?
 H21A C21 H21B 108.0 . . ?
 C22 C21 H21A 109.3 . . ?
 C22 C21 H21B 109.3 . . ?
 C21 C22 H22A 109.4 . . ?
 C21 C22 H22B 109.4 . . ?
 C21 C22 C23 111.3(2) . . ?
 H22A C22 H22B 108.0 . . ?
 C23 C22 H22A 109.4 . . ?
 C23 C22 H22B 109.4 . . ?
 C18 C23 C22 110.1(2) . . ?
 C18 C23 H23A 109.6 . . ?
 C18 C23 H23B 109.6 . . ?
 C22 C23 H23A 109.6 . . ?
 C22 C23 H23B 109.6 . . ?
 H23A C23 H23B 108.2 . . ?
 O8 S2 O9 114.64(15) . . ?
 O8 S2 C24 103.37(15) . . ?
 O9 S2 C24 102.13(14) . . ?
 O10 S2 O8 115.11(14) . . ?
 O10 S2 O9 114.65(15) . . ?
 O10 S2 C24 104.69(16) . . ?
 F4 C24 S2 110.4(2) . . ?
 F5 C24 S2 110.4(2) . . ?
 F5 C24 F4 107.7(3) . . ?
 F6 C24 S2 111.2(2) . . ?
 F6 C24 F4 107.4(3) . . ?
 F6 C24 F5 109.7(3) . . ?
 C25 O11 H11A 123(2) . . ?
 O11 C25 H25 108.3 . . ?
 O11 C25 C26 108.2(3) . . ?
 O11 C25 C30 111.2(3) . . ?
 C26 C25 H25 108.3 . . ?
 C30 C25 H25 108.3 . . ?
 C30 C25 C26 112.3(3) . . ?
 C25 C26 H26A 108.8 . . ?
 C25 C26 H26B 108.8 . . ?
 H26A C26 H26B 107.7 . . ?
 C27 C26 C25 113.8(4) . . ?
 C27 C26 H26A 108.8 . . ?
 C27 C26 H26B 108.8 . . ?
 C26 C27 H27A 109.2 . . ?
 C26 C27 H27B 109.2 . . ?
 C26 C27 C28 112.0(4) . . ?
 H27A C27 H27B 107.9 . . ?
 C28 C27 H27A 109.2 . . ?
 C28 C27 H27B 109.2 . . ?
 C27 C28 H28A 109.6 . . ?
 C27 C28 H28B 109.6 . . ?
 C27 C28 C29 110.3(4) . . ?
 H28A C28 H28B 108.1 . . ?
 C29 C28 H28A 109.6 . . ?
 C29 C28 H28B 109.6 . . ?
 C28 C29 H29A 109.4 . . ?
 C28 C29 H29B 109.4 . . ?
 H29A C29 H29B 108.0 . . ?
 C30 C29 C28 111.2(4) . . ?
 C30 C29 H29A 109.4 . . ?
 C30 C29 H29B 109.4 . . ?
 C25 C30 C29 110.6(4) . . ?
 C25 C30 H30A 109.5 . . ?
 C25 C30 H30B 109.5 . . ?
 C29 C30 H30A 109.5 . . ?
 C29 C30 H30B 109.5 . . ?
 H30A C30 H30B 108.1 . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O1 H1 O11 0.92(4) 1.69(4) 2.575(3) 161(4) . yes
 O7 H7 O8 0.95(6) 1.80(6) 2.735(3) 168(5) . yes
 O11 H11A O9 0.93(4) 1.83(4) 2.744(3) 167(4) . yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Fe1 O1 C1 C2 47.4(2) . . . . ?
 Fe1 O7 C18 C19 -141.61(19) . . . . ?
 Fe1 O7 C18 C23 94.4(2) . . . . ?
 Fe1 N1 C2 C1 9.9(2) . . . . ?
 Fe1 N1 C2 C3 -111.29(16) . . . . ?
 Fe1 N1 C2 C5 132.35(15) . . . . ?
 Fe1 N1 C4 O2 138.66(14) . . . . ?
 Fe1 N1 C4 C7 18.9(2) . . . . ?
 Fe1 N1 C6 O3 -154.99(14) . . . . ?
 Fe1 N1 C6 C12 -36.3(2) . . . . ?
 Fe1 N2 C7 C4 9.1(3) . . . . ?
 Fe1 N2 C7 C8 -172.06(18) . . . . ?
 Fe1 N2 C11 C10 173.6(2) . . . . ?
 Fe1 N3 C12 C6 1.4(3) . . . . ?
 Fe1 N3 C12 C13 179.0(2) . . . . ?
 Fe1 N3 C16 C15 -176.9(2) . . . . ?
 O1 C1 C2 N1 -35.8(3) . . . . ?
 O1 C1 C2 C3 79.0(2) . . . . ?
 O1 C1 C2 C5 -152.3(2) . . . . ?
 O2 C4 C7 N2 -137.0(2) . . . . ?
 O2 C4 C7 C8 44.2(3) . . . . ?
 O3 C6 C12 N3 140.2(2) . . . . ?
 O3 C6 C12 C13 -37.5(3) . . . . ?
 O4 S1 C17 F1 179.6(2) . . . . ?
 O4 S1 C17 F2 -60.1(2) . . . . ?
 O4 S1 C17 F3 59.9(2) . . . . ?
 O5 S1 O4 Fe1 -23.1(4) . . . . ?
 O5 S1 C17 F1 59.5(2) . . . . ?
 O5 S1 C17 F2 179.8(2) . . . . ?
 O5 S1 C17 F3 -60.2(2) . . . . ?
 O6 S1 O4 Fe1 113.7(3) . . . . ?
 O6 S1 C17 F1 -63.1(2) . . . . ?
 O6 S1 C17 F2 57.1(2) . . . . ?
 O6 S1 C17 F3 177.2(2) . . . . ?
 O7 C18 C19 C20 179.7(2) . . . . ?
 O7 C18 C23 C22 -179.9(2) . . . . ?
 N1 C2 C3 O2 -33.6(2) . . . . ?
 N1 C2 C5 O3 9.3(2) . . . . ?
 N1 C4 C7 N2 -18.9(3) . . . . ?
 N1 C4 C7 C8 162.3(2) . . . . ?
 N1 C6 C12 N3 24.4(3) . . . . ?
 N1 C6 C12 C13 -153.3(2) . . . . ?
 N2 C7 C8 C9 -1.8(4) . . . . ?
 N3 C12 C13 C14 -1.9(4) . . . . ?
 C1 C2 C3 O2 -153.89(19) . . . . ?
 C1 C2 C5 O3 130.5(2) . . . . ?
 C2 N1 C4 O2 16.5(2) . . . . ?
 C2 N1 C4 C7 -103.3(2) . . . . ?
 C2 N1 C6 O3 -35.0(2) . . . . ?
 C2 N1 C6 C12 83.7(2) . . . . ?
 C3 O2 C4 N1 -38.5(2) . . . . ?
 C3 O2 C4 C7 82.5(2) . . . . ?
 C3 C2 C5 O3 -100.2(2) . . . . ?
 C4 O2 C3 C2 44.8(2) . . . . ?
 C4 N1 C2 C1 131.6(2) . . . . ?
 C4 N1 C2 C3 10.4(2) . . . . ?
 C4 N1 C2 C5 -105.9(2) . . . . ?
 C4 N1 C6 O3 79.0(2) . . . . ?
 C4 N1 C6 C12 -162.35(19) . . . . ?
 C4 C7 C8 C9 176.9(2) . . . . ?
 C5 O3 C6 N1 41.9(2) . . . . ?
 C5 O3 C6 C12 -76.4(2) . . . . ?
 C5 C2 C3 O2 76.6(2) . . . . ?
 C6 O3 C5 C2 -31.2(2) . . . . ?
 C6 N1 C2 C1 -107.5(2) . . . . ?
 C6 N1 C2 C3 131.25(18) . . . . ?
 C6 N1 C2 C5 14.9(2) . . . . ?
 C6 N1 C4 O2 -97.0(2) . . . . ?
 C6 N1 C4 C7 143.26(19) . . . . ?
 C6 C12 C13 C14 175.7(2) . . . . ?
 C7 N2 C11 C10 -1.1(4) . . . . ?
 C7 C8 C9 C10 -1.2(4) . . . . ?
 C8 C9 C10 C11 3.0(4) . . . . ?
 C9 C10 C11 N2 -1.9(4) . . . . ?
 C11 N2 C7 C4 -175.8(2) . . . . ?
 C11 N2 C7 C8 3.0(4) . . . . ?
 C12 N3 C16 C15 0.9(4) . . . . ?
 C12 C13 C14 C15 1.0(4) . . . . ?
 C13 C14 C15 C16 0.7(5) . . . . ?
 C14 C15 C16 N3 -1.7(4) . . . . ?
 C16 N3 C12 C6 -176.7(2) . . . . ?
 C16 N3 C12 C13 1.0(4) . . . . ?
 C17 S1 O4 Fe1 -136.0(3) . . . . ?
 C18 C19 C20 C21 54.9(3) . . . . ?
 C19 C18 C23 C22 57.4(3) . . . . ?
 C19 C20 C21 C22 -54.3(4) . . . . ?
 C20 C21 C22 C23 54.9(4) . . . . ?
 C21 C22 C23 C18 -55.8(3) . . . . ?
 C23 C18 C19 C20 -57.0(3) . . . . ?
 O8 S2 C24 F4 -177.5(2) . . . . ?
 O8 S2 C24 F5 63.5(3) . . . . ?
 O8 S2 C24 F6 -58.5(3) . . . . ?
 O9 S2 C24 F4 -58.2(2) . . . . ?
 O9 S2 C24 F5 -177.2(3) . . . . ?
 O9 S2 C24 F6 60.8(3) . . . . ?
 O10 S2 C24 F4 61.6(2) . . . . ?
 O10 S2 C24 F5 -57.3(3) . . . . ?
 O10 S2 C24 F6 -179.4(2) . . . . ?
 O11 C25 C26 C27 68.7(4) . . . . ?
 O11 C25 C30 C29 -66.9(4) . . . . ?
 C25 C26 C27 C28 53.3(5) . . . . ?
 C26 C25 C30 C29 54.5(5) . . . . ?
 C26 C27 C28 C29 -52.8(6) . . . . ?
 C27 C28 C29 C30 54.2(6) . . . . ?
 C28 C29 C30 C25 -55.3(6) . . . . ?
 C30 C25 C26 C27 -54.4(5) . . . . ?


_olex2_submission_original_sample_id  jonon94
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  2.577
_oxdiff_exptl_absorpt_empirical_full_min  0.490
#===END
data_C

_vrf_PLAT302_jonon101
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 88% 
         _G Anion/Solvent/Minor-Residue Disorder (Resd  3  ) .. 50% 
RESPONSE: Triflate anions containing S1 and S2 are modeled as
disordered over two positions (0.57(3):0.43(3) and 0.503(2):0.497(2),
respectively).
;

_vrf_PLAT860_jonon101
;
PROBLEM: _G Number of Least-Squares Restraints ............. 306 
RESPONSE: Analogous bond lengths and angles between the two
positions of each triflate anion were restrained to be similar.
Anisotropic displacement parameters between proximal atoms were
restrained to be similar and restrained toward the expected
thermal motion relative to bond direction.
;

_audit_creation_date               2020-11-11
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

#CrysAlisPro, version 171.40.84a
Rigaku Oxford Diffraction (2020). CrysAlisPro Software system,
version 171.40.84a. Rigaku Corporation, Oxford, UK.

#SHELXT-2018/2
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3--8.

#SHELXL-2018/3
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3--8.
;
_publ_contact_author_name        'William D. Jones'
_publ_contact_author_address     
;
 'Department of Chemistry, University of Rochester, Rochester, New York 14627'
;
_publ_contact_author_email       'jones@chem.rochester.edu'
_publ_requested_journal          'J. Am. Chem. Soc.'
_publ_section_title            
;
Iron-Based Dehydration Catalyst for Selective Formation of Styrene
;

loop_
_publ_author_name                
 'Olaf Nachtigall'
 'Andrew I. VanderWeide'
 'William W. Brennessel'
 'William D. Jones'

_publ_author_address             
;
 Department of Chemistry, University of Rochester, Rochester, NY  14627 USA
;

_chemical_name_common              jonon101
_chemical_name_systematic          '[(FOX)Fe(H2O)2][OTf]2'
_chemical_formula_moiety           'C16 H21 Fe N3 O5, 2(C F3 O3 S)'
_chemical_formula_sum              'C18 H21 F6 Fe N3 O11 S2'
_chemical_formula_weight           689.35
_chemical_melting_point            ?
_chemical_oxdiff_formula           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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'
 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe' 'Fe' -1.1336 3.1974
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'monoclinic'
_space_group_IT_number             14
_space_group_name_H-M_alt          'P 1 21/c 1'
_space_group_name_Hall             '-P 2ybc'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'

_cell_length_a                     13.3968(2)
_cell_length_b                     9.43800(10)
_cell_length_c                     20.5184(3)
_cell_angle_alpha                  90
_cell_angle_beta                   100.509(2)
_cell_angle_gamma                  90
_cell_volume                       2550.81(6)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      20479
_cell_measurement_temperature      100.00(10)
_cell_measurement_theta_max        77.7400
_cell_measurement_theta_min        3.3440
_shelx_estimated_absorpt_T_max     0.619
_shelx_estimated_absorpt_T_min     0.318
_exptl_absorpt_coefficient_mu      7.280
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.56339
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      1.795
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1400
_exptl_crystal_size_max            0.204
_exptl_crystal_size_mid            0.107
_exptl_crystal_size_min            0.073
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0449
_diffrn_reflns_av_unetI/netI       0.0279
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.991
_diffrn_reflns_limit_h_max         16
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         11
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         24
_diffrn_reflns_limit_l_min         -26
_diffrn_reflns_number              33019
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.991
_diffrn_reflns_theta_full          74.504
_diffrn_reflns_theta_max           77.699
_diffrn_reflns_theta_min           3.355
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        100.00(10)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     33.00 121.00   0.50    0.20    --   49.87  69.00 129.00  176
  2  ω     89.00 178.00   0.50    0.80    --  105.75  69.00 129.00  178
  3  ω     98.00 164.00   0.50    0.80    --  105.75  15.00 150.00  132
  4  ω     98.00 164.00   0.50    0.80    --  105.75  15.00  90.00  132
  5  ω     98.00 164.00   0.50    0.80    --  105.75  15.00  60.00  132
  6  ω     92.00 178.00   0.50    0.80    --  105.75  61.00  60.00  172
  7  ω     97.00 178.00   0.50    0.80    --  105.75  45.00-120.00  162
  8  ω     98.00 164.00   0.50    0.80    --  105.75  15.00-150.00  132
  9  ω    -42.00 -12.00   0.50    0.80    --  -84.25  45.00 -90.00   60
 10  ω    -67.00  22.00   0.50    0.20    --  -49.87  69.00 129.00  178
 11  ω     34.00 116.00   0.50    0.80    --  105.75-125.00 150.00  164
 12  ω     34.00 116.00   0.50    0.80    --  105.75-125.00  30.00  164
 13  ω   -101.00 -12.00   0.50    0.80    --  -84.25  69.00 129.00  178
 14  ω   -121.00 -70.00   0.50    0.20    --  -49.87-125.00 -90.00  102
 15  ω   -121.00 -33.00   0.50    0.20    --  -49.87 -69.00  -3.00  176
 16  ω    -21.00  67.00   0.50    0.20    --   49.87 -69.00  -3.00  176
 17  ω    -22.00   5.00   0.50    0.20    --   49.87 -19.00-120.00   54
 18  ω    -22.00   5.00   0.50    0.20    --   49.87 -19.00-150.00   54
 19  ω    -22.00   5.00   0.50    0.20    --   49.87 -19.00   0.00   54
 20  ω     34.00  87.00   0.50    0.80    --  105.75 -61.00-120.00  106
 21  ω     34.00 127.00   0.50    0.80    --  105.75 -77.00-180.00  186
 22  ω     34.00  87.00   0.50    0.80    --  105.75 -61.00 -60.00  106
 23  ω     34.00  87.00   0.50    0.80    --  105.75 -61.00 -90.00  106
 24  ω     34.00 123.00   0.50    0.80    --  105.75 -69.00  -3.00  178
 25  ω     34.00  87.00   0.50    0.80    --  105.75 -61.00  30.00  106
 26  ω     34.00  87.00   0.50    0.80    --  105.75 -61.00 150.00  106
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0696318000
_diffrn_orient_matrix_UB_12        0.0579817000
_diffrn_orient_matrix_UB_13        -0.0623790000
_diffrn_orient_matrix_UB_21        0.0799381000
_diffrn_orient_matrix_UB_22        0.1134556000
_diffrn_orient_matrix_UB_23        -0.0071843000
_diffrn_orient_matrix_UB_31        0.0493743000
_diffrn_orient_matrix_UB_32        -0.1020273000
_diffrn_orient_matrix_UB_33        -0.0434549000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Cu K\a'
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  5089
_reflns_number_total               5380
_reflns_odcompleteness_completeness  100.00
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max           0.327
_refine_diff_density_min           -0.514
_refine_diff_density_rms           0.065
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.084
_refine_ls_hydrogen_treatment      mixed
_refine_ls_matrix_type             full
_refine_ls_number_parameters       491
_refine_ls_number_reflns           5380
_refine_ls_number_restraints       306
_refine_ls_R_factor_all            0.0325
_refine_ls_R_factor_gt             0.0306
_refine_ls_restrained_S_all        1.069
_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)+(0.0435P)²+1.4330P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0814
_refine_ls_wR_factor_ref           0.0825
_refine_special_details 
;
Triflate anions containing S1 and S2 are modeled as disordered
over two positions (0.57(3):0.43(3) and 0.503(2):0.497(2),
respectively). Analogous bond lengths and angles between the two
positions of each triflate anion were restrained to be similar.
Anisotropic displacement parameters between proximal atoms were
restrained to be similar and restrained toward the expected
thermal motion relative to bond direction.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S2-C18 \\sim S2-C18'
 with sigma of 0.01
 S2-O9 \\sim S2-O10 \\sim S2-O11 \\sim S2-O9' \\sim S2-O10' \\sim S2-O11'
 with sigma of 0.01
 O9-O10 \\sim O10-O11 \\sim O11-O9 \\sim O9'-O10' \\sim O10'-O11' \\sim O11'-O9'
 with sigma of 0.02
 C18-F4 \\sim C18-F5 \\sim C18-F6 \\sim C18'-F4' \\sim C18'-F5' \\sim C18'-F6'
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4'-F5' \\sim F5'-F6' \\sim F6'-F4'
 with sigma of 0.02
 S1-C17 \\sim S1-C17'
 with sigma of 0.01
 C17-F1 \\sim C17-F2 \\sim C17-F3 \\sim C17'-F1' \\sim C17'-F2' \\sim C17'-F3'
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1'-F2' \\sim F2'-F3' \\sim F3'-F1'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
4. Rigid body (RIGU) restrains
 S2, F4, F5, F6, O9, O10, O11, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, F4', F5', F6', O9', O10', O11', C18'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1, F2, F3, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1', F2', F3', C17'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4')=Sof(F5')=Sof(F6')=Sof(O9')=Sof(O10')=Sof(O11')=Sof(C18')=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(C18)=FVAR(1)
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(C17')=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C17)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5C,H5D)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap
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
 Fe1 Fe 0.31595(2) 0.53902(3) 0.71866(2) 0.01320(8) Uani 1 1 d . . . . .
 O1 O 0.23598(9) 0.35951(14) 0.74847(7) 0.0207(3) Uani 1 1 d . . . . .
 H1 H 0.257(2) 0.280(3) 0.7564(14) 0.041(8) Uiso 1 1 d . . . . .
 O2 O 0.00980(9) 0.69823(13) 0.68159(6) 0.0197(3) Uani 1 1 d . . . . .
 O3 O 0.09519(9) 0.66392(14) 0.83251(6) 0.0218(3) Uani 1 1 d . . . . .
 O4 O 0.42253(10) 0.39494(14) 0.69972(7) 0.0217(3) Uani 1 1 d . . . . .
 H4A H 0.476(3) 0.407(4) 0.6845(17) 0.066(10) Uiso 1 1 d . . . . .
 H4B H 0.397(2) 0.317(4) 0.6852(15) 0.049(8) Uiso 1 1 d . . . . .
 O5 O 0.40533(10) 0.71005(15) 0.69340(7) 0.0231(3) Uani 1 1 d . . . . .
 H5A H 0.470(3) 0.717(3) 0.7012(15) 0.053(9) Uiso 1 1 d . . . . .
 H5B H 0.379(2) 0.781(3) 0.6724(14) 0.040(7) Uiso 1 1 d . . . . .
 N1 N 0.16591(10) 0.62247(14) 0.73845(7) 0.0138(3) Uani 1 1 d . . . . .
 N2 N 0.22312(11) 0.56424(15) 0.62144(7) 0.0161(3) Uani 1 1 d . . . . .
 N3 N 0.35245(11) 0.60348(16) 0.81899(7) 0.0171(3) Uani 1 1 d . . . . .
 C1 C 0.12912(13) 0.36248(18) 0.72473(10) 0.0200(3) Uani 1 1 d . . . . .
 H1A H 0.096265 0.285739 0.744140 0.024 Uiso 1 1 calc R U . . .
 H1B H 0.114581 0.352222 0.676894 0.024 Uiso 1 1 calc R U . . .
 C2 C 0.09080(12) 0.50533(18) 0.74494(9) 0.0163(3) Uani 1 1 d . . . . .
 C3 C -0.00770(13) 0.55417(19) 0.69827(10) 0.0206(4) Uani 1 1 d . . . . .
 H3A H -0.020816 0.495836 0.658707 0.025 Uiso 1 1 calc R U . . .
 H3B H -0.065440 0.547750 0.720581 0.025 Uiso 1 1 calc R U . . .
 C4 C 0.11567(12) 0.70544(18) 0.68143(8) 0.0159(3) Uani 1 1 d . . . . .
 H4 H 0.138634 0.804127 0.685955 0.019 Uiso 1 1 calc R U . . .
 C5 C 0.08108(14) 0.5159(2) 0.81827(9) 0.0213(4) Uani 1 1 d . . . . .
 H5C H 0.014689 0.484457 0.824833 0.026 Uiso 1 1 calc R U . . .
 H5D H 0.132796 0.459690 0.845991 0.026 Uiso 1 1 calc R U . . .
 C6 C 0.17939(13) 0.69969(18) 0.80263(8) 0.0171(3) Uani 1 1 d . . . . .
 H6 H 0.179639 0.801995 0.794491 0.021 Uiso 1 1 calc R U . . .
 C7 C 0.13874(12) 0.64267(18) 0.61739(8) 0.0161(3) Uani 1 1 d . . . . .
 C8 C 0.07447(14) 0.6701(2) 0.55760(9) 0.0212(4) Uani 1 1 d . . . . .
 H8 H 0.016075 0.724096 0.556362 0.025 Uiso 1 1 calc R U . . .
 C9 C 0.09892(14) 0.6157(2) 0.49990(9) 0.0250(4) Uani 1 1 d . . . . .
 H9 H 0.057726 0.633947 0.459159 0.030 Uiso 1 1 calc R U . . .
 C10 C 0.18568(15) 0.5335(2) 0.50358(9) 0.0233(4) Uani 1 1 d . . . . .
 H10 H 0.203193 0.494635 0.465557 0.028 Uiso 1 1 calc R U . . .
 C11 C 0.24561(14) 0.5107(2) 0.56525(9) 0.0201(3) Uani 1 1 d . . . . .
 H11 H 0.303923 0.455987 0.567811 0.024 Uiso 1 1 calc R U . . .
 C12 C 0.27813(13) 0.65675(18) 0.84747(8) 0.0166(3) Uani 1 1 d . . . . .
 C13 C 0.29090(14) 0.6790(2) 0.91534(9) 0.0220(4) Uani 1 1 d . . . . .
 H13 H 0.237519 0.712579 0.934303 0.026 Uiso 1 1 calc R U . . .
 C14 C 0.38435(16) 0.6504(2) 0.95436(9) 0.0259(4) Uani 1 1 d . . . . .
 H14 H 0.394322 0.663460 1.000018 0.031 Uiso 1 1 calc R U . . .
 C15 C 0.46278(15) 0.6021(2) 0.92470(10) 0.0262(4) Uani 1 1 d . . . . .
 H15 H 0.527001 0.586019 0.949668 0.031 Uiso 1 1 calc R U . . .
 C16 C 0.44344(14) 0.5783(2) 0.85717(9) 0.0218(4) Uani 1 1 d . . . . .
 H16 H 0.495497 0.543468 0.837271 0.026 Uiso 1 1 calc R U . . .
 S1 S 0.25297(3) 0.05333(4) 0.62956(2) 0.02062(11) Uani 1 1 d D . . . .
 O6 O 0.31890(11) 0.17458(15) 0.63463(7) 0.0307(3) Uani 1 1 d . . . . .
 O7 O 0.30042(12) -0.07822(16) 0.61650(8) 0.0334(3) Uani 1 1 d . . . . .
 O8 O 0.18866(13) 0.04572(17) 0.67824(9) 0.0390(4) Uani 1 1 d . . . . .
 F1 F 0.1094(10) -0.0195(6) 0.5278(9) 0.060(3) Uani 0.57(3) 1 d D U P A 1
 F2 F 0.1187(12) 0.2006(12) 0.5551(9) 0.053(2) Uani 0.57(3) 1 d D U P A 1
 F3 F 0.2250(10) 0.1121(10) 0.5003(4) 0.0470(16) Uani 0.57(3) 1 d D U P A 1
 C17 C 0.1734(9) 0.0852(8) 0.5483(4) 0.031(2) Uani 0.57(3) 1 d D U P A 1
 F1' F 0.0845(8) -0.0096(7) 0.5534(8) 0.044(2) Uani 0.43(3) 1 d D U P A 2
 F2' F 0.1095(13) 0.2158(11) 0.5573(9) 0.039(2) Uani 0.43(3) 1 d D U P A 2
 F3' F 0.1965(12) 0.081(2) 0.5037(5) 0.049(2) Uani 0.43(3) 1 d D U P A 2
 C17' C 0.1543(8) 0.0904(10) 0.5569(4) 0.024(2) Uani 0.43(3) 1 d D U P A 2
 S2 S 0.35391(3) 0.06183(4) 0.84713(2) 0.01648(10) Uani 1 1 d D . . . .
 F4 F 0.52033(16) 0.1083(3) 0.93059(12) 0.0356(7) Uani 0.503(2) 1 d D . P B 1
 F5 F 0.4072(2) -0.0068(4) 0.97161(12) 0.0466(8) Uani 0.503(2) 1 d D . P B 1
 F6 F 0.3887(3) 0.2147(4) 0.9524(2) 0.0558(11) Uani 0.503(2) 1 d D U P B 1
 O9 O 0.2483(5) 0.0566(11) 0.8521(7) 0.0217(18) Uani 0.503(2) 1 d D U P B 1
 O10 O 0.3819(6) 0.1749(5) 0.8070(3) 0.0249(13) Uani 0.503(2) 1 d D U P B 1
 O11 O 0.3956(2) -0.0751(3) 0.83191(18) 0.0242(6) Uani 0.503(2) 1 d D U P B 1
 C18 C 0.4212(3) 0.0959(4) 0.93014(18) 0.0290(9) Uani 0.503(2) 1 d D U P B 1
 F4' F 0.47264(19) 0.2529(3) 0.91760(12) 0.0392(7) Uani 0.497(2) 1 d D . P B 2
 F5' F 0.3758(2) 0.1411(4) 0.97325(13) 0.0371(8) Uani 0.497(2) 1 d D U P B 2
 F6' F 0.3137(2) 0.3028(3) 0.90312(13) 0.0371(7) Uani 0.497(2) 1 d D . P B 2
 O9' O 0.2505(5) 0.0251(11) 0.8475(8) 0.0218(17) Uani 0.497(2) 1 d D U P B 2
 O10' O 0.3733(6) 0.1429(6) 0.7909(2) 0.0216(12) Uani 0.497(2) 1 d D U P B 2
 O11' O 0.4284(2) -0.0439(3) 0.87003(18) 0.0258(7) Uani 0.497(2) 1 d D U P B
 2
 C18' C 0.3807(3) 0.1964(4) 0.9137(2) 0.0262(9) Uani 0.497(2) 1 d D U P B 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Fe1 O1 2.1521(13) . ?
 Fe1 O4 2.0594(13) . ?
 Fe1 O5 2.1295(13) . ?
 Fe1 N1 2.2636(13) . ?
 Fe1 N2 2.1627(15) . ?
 Fe1 N3 2.1167(15) . ?
 O1 H1 0.81(3) . ?
 O1 C1 1.426(2) . ?
 O2 C3 1.432(2) . ?
 O2 C4 1.4205(19) . ?
 O3 C5 1.433(2) . ?
 O3 C6 1.419(2) . ?
 O4 H4A 0.84(4) . ?
 O4 H4B 0.84(3) . ?
 O5 H5A 0.85(3) . ?
 O5 H5B 0.84(3) . ?
 N1 C2 1.517(2) . ?
 N1 C4 1.466(2) . ?
 N1 C6 1.487(2) . ?
 N2 C7 1.341(2) . ?
 N2 C11 1.342(2) . ?
 N3 C12 1.341(2) . ?
 N3 C16 1.344(2) . ?
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C2 1.527(2) . ?
 C2 C3 1.552(2) . ?
 C2 C5 1.537(2) . ?
 C3 H3A 0.9700 . ?
 C3 H3B 0.9700 . ?
 C4 H4 0.9800 . ?
 C4 C7 1.524(2) . ?
 C5 H5C 0.9700 . ?
 C5 H5D 0.9700 . ?
 C6 H6 0.9800 . ?
 C6 C12 1.522(2) . ?
 C7 C8 1.389(2) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.384(3) . ?
 C9 H9 0.9300 . ?
 C9 C10 1.388(3) . ?
 C10 H10 0.9300 . ?
 C10 C11 1.386(3) . ?
 C11 H11 0.9300 . ?
 C12 C13 1.388(2) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.384(3) . ?
 C14 H14 0.9300 . ?
 C14 C15 1.384(3) . ?
 C15 H15 0.9300 . ?
 C15 C16 1.381(3) . ?
 C16 H16 0.9300 . ?
 S1 O6 1.4377(14) . ?
 S1 O7 1.4420(15) . ?
 S1 O8 1.4349(16) . ?
 S1 C17 1.833(5) . ?
 S1 C17' 1.837(6) . ?
 F1 C17 1.326(5) . ?
 F2 C17 1.333(5) . ?
 F3 C17 1.327(6) . ?
 F1' C17' 1.321(6) . ?
 F2' C17' 1.328(6) . ?
 F3' C17' 1.320(6) . ?
 S2 O9 1.438(5) . ?
 S2 O10 1.439(4) . ?
 S2 O11 1.463(3) . ?
 S2 C18 1.805(4) . ?
 S2 O9' 1.429(5) . ?
 S2 O10' 1.446(5) . ?
 S2 O11' 1.429(3) . ?
 S2 C18' 1.852(5) . ?
 F4 C18 1.331(4) . ?
 F5 C18 1.325(4) . ?
 F6 C18 1.315(4) . ?
 F4' C18' 1.332(4) . ?
 F5' C18' 1.341(4) . ?
 F6' C18' 1.338(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
 O1 Fe1 N1 73.65(5) . . ?
 O1 Fe1 N2 96.69(5) . . ?
 O4 Fe1 O1 86.11(5) . . ?
 O4 Fe1 O5 90.84(6) . . ?
 O4 Fe1 N1 158.84(5) . . ?
 O4 Fe1 N2 101.57(6) . . ?
 O4 Fe1 N3 109.16(6) . . ?
 O5 Fe1 O1 175.67(5) . . ?
 O5 Fe1 N1 109.70(5) . . ?
 O5 Fe1 N2 86.93(5) . . ?
 N2 Fe1 N1 75.35(5) . . ?
 N3 Fe1 O1 89.34(5) . . ?
 N3 Fe1 O5 88.76(6) . . ?
 N3 Fe1 N1 77.33(5) . . ?
 N3 Fe1 N2 149.02(6) . . ?
 Fe1 O1 H1 128(2) . . ?
 C1 O1 Fe1 114.10(10) . . ?
 C1 O1 H1 112(2) . . ?
 C4 O2 C3 104.66(13) . . ?
 C6 O3 C5 103.27(12) . . ?
 Fe1 O4 H4A 131(3) . . ?
 Fe1 O4 H4B 113(2) . . ?
 H4A O4 H4B 108(3) . . ?
 Fe1 O5 H5A 127(2) . . ?
 Fe1 O5 H5B 122(2) . . ?
 H5A O5 H5B 111(3) . . ?
 C2 N1 Fe1 112.77(10) . . ?
 C4 N1 Fe1 109.65(9) . . ?
 C4 N1 C2 104.13(12) . . ?
 C4 N1 C6 114.14(13) . . ?
 C6 N1 Fe1 111.17(10) . . ?
 C6 N1 C2 104.76(12) . . ?
 C7 N2 Fe1 117.03(11) . . ?
 C7 N2 C11 118.24(15) . . ?
 C11 N2 Fe1 124.70(12) . . ?
 C12 N3 Fe1 118.26(12) . . ?
 C12 N3 C16 118.61(15) . . ?
 C16 N3 Fe1 122.68(12) . . ?
 O1 C1 H1A 110.3 . . ?
 O1 C1 H1B 110.3 . . ?
 O1 C1 C2 106.91(14) . . ?
 H1A C1 H1B 108.6 . . ?
 C2 C1 H1A 110.3 . . ?
 C2 C1 H1B 110.3 . . ?
 N1 C2 C1 111.01(13) . . ?
 N1 C2 C3 103.43(13) . . ?
 N1 C2 C5 102.40(13) . . ?
 C1 C2 C3 112.63(14) . . ?
 C1 C2 C5 114.57(15) . . ?
 C5 C2 C3 111.74(14) . . ?
 O2 C3 C2 105.76(14) . . ?
 O2 C3 H3A 110.6 . . ?
 O2 C3 H3B 110.6 . . ?
 C2 C3 H3A 110.6 . . ?
 C2 C3 H3B 110.6 . . ?
 H3A C3 H3B 108.7 . . ?
 O2 C4 N1 106.61(13) . . ?
 O2 C4 H4 110.0 . . ?
 O2 C4 C7 110.06(13) . . ?
 N1 C4 H4 110.0 . . ?
 N1 C4 C7 110.18(13) . . ?
 C7 C4 H4 110.0 . . ?
 O3 C5 C2 103.37(14) . . ?
 O3 C5 H5C 111.1 . . ?
 O3 C5 H5D 111.1 . . ?
 C2 C5 H5C 111.1 . . ?
 C2 C5 H5D 111.1 . . ?
 H5C C5 H5D 109.1 . . ?
 O3 C6 N1 106.75(13) . . ?
 O3 C6 H6 109.6 . . ?
 O3 C6 C12 110.31(14) . . ?
 N1 C6 H6 109.6 . . ?
 N1 C6 C12 110.89(13) . . ?
 C12 C6 H6 109.6 . . ?
 N2 C7 C4 117.54(14) . . ?
 N2 C7 C8 122.52(16) . . ?
 C8 C7 C4 119.92(15) . . ?
 C7 C8 H8 120.6 . . ?
 C9 C8 C7 118.77(17) . . ?
 C9 C8 H8 120.6 . . ?
 C8 C9 H9 120.4 . . ?
 C8 C9 C10 119.19(17) . . ?
 C10 C9 H9 120.4 . . ?
 C9 C10 H10 120.8 . . ?
 C11 C10 C9 118.43(17) . . ?
 C11 C10 H10 120.8 . . ?
 N2 C11 C10 122.84(17) . . ?
 N2 C11 H11 118.6 . . ?
 C10 C11 H11 118.6 . . ?
 N3 C12 C6 117.97(15) . . ?
 N3 C12 C13 121.91(16) . . ?
 C13 C12 C6 120.06(15) . . ?
 C12 C13 H13 120.5 . . ?
 C14 C13 C12 118.95(17) . . ?
 C14 C13 H13 120.5 . . ?
 C13 C14 H14 120.4 . . ?
 C13 C14 C15 119.27(17) . . ?
 C15 C14 H14 120.4 . . ?
 C14 C15 H15 120.8 . . ?
 C16 C15 C14 118.45(18) . . ?
 C16 C15 H15 120.8 . . ?
 N3 C16 C15 122.69(17) . . ?
 N3 C16 H16 118.7 . . ?
 C15 C16 H16 118.7 . . ?
 O6 S1 O7 114.39(10) . . ?
 O6 S1 C17 100.5(2) . . ?
 O6 S1 C17' 104.4(3) . . ?
 O7 S1 C17 100.1(4) . . ?
 O7 S1 C17' 106.8(4) . . ?
 O8 S1 O6 115.37(10) . . ?
 O8 S1 O7 115.29(10) . . ?
 O8 S1 C17 108.5(5) . . ?
 O8 S1 C17' 98.0(4) . . ?
 F1 C17 S1 113.7(5) . . ?
 F1 C17 F2 107.8(7) . . ?
 F1 C17 F3 107.5(5) . . ?
 F2 C17 S1 106.1(10) . . ?
 F3 C17 S1 114.3(6) . . ?
 F3 C17 F2 107.0(7) . . ?
 F1' C17' S1 107.8(5) . . ?
 F1' C17' F2' 108.7(8) . . ?
 F2' C17' S1 115.1(11) . . ?
 F3' C17' S1 107.7(7) . . ?
 F3' C17' F1' 108.2(7) . . ?
 F3' C17' F2' 109.1(8) . . ?
 O9 S2 O10 115.4(5) . . ?
 O9 S2 O11 113.8(4) . . ?
 O9 S2 C18 105.5(6) . . ?
 O10 S2 O11 112.6(3) . . ?
 O10 S2 C18 105.7(3) . . ?
 O11 S2 C18 102.36(19) . . ?
 O9' S2 O10' 116.6(6) . . ?
 O9' S2 O11' 116.7(5) . . ?
 O9' S2 C18' 102.7(6) . . ?
 O10' S2 C18' 100.7(2) . . ?
 O11' S2 O10' 114.6(4) . . ?
 O11' S2 C18' 101.9(2) . . ?
 F4 C18 S2 110.4(2) . . ?
 F5 C18 S2 111.8(3) . . ?
 F5 C18 F4 108.5(3) . . ?
 F6 C18 S2 109.9(3) . . ?
 F6 C18 F4 108.4(3) . . ?
 F6 C18 F5 107.8(4) . . ?
 F4' C18' S2 111.8(3) . . ?
 F4' C18' F5' 107.4(3) . . ?
 F4' C18' F6' 107.2(3) . . ?
 F5' C18' S2 111.7(3) . . ?
 F6' C18' S2 111.2(3) . . ?
 F6' C18' F5' 107.3(4) . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O1 H1 O10 0.81(3) 2.05(3) 2.728(7) 140(3) . yes
 O1 H1 O10' 0.81(3) 2.05(3) 2.782(8) 150(3) . yes
 O4 H4A O11 0.84(4) 1.82(4) 2.649(3) 169(3) 2_656 yes
 O4 H4A O11' 0.84(4) 1.90(4) 2.722(3) 164(3) 2_656 yes
 O4 H4B O6 0.84(3) 1.89(3) 2.713(2) 165(3) . yes
 O5 H5A O10 0.85(3) 2.06(3) 2.871(8) 158(3) 2_656 yes
 O5 H5A O10' 0.85(3) 2.19(3) 2.992(8) 156(3) 2_656 yes
 O5 H5B O7 0.84(3) 1.94(3) 2.766(2) 170(3) 1_565 yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Fe1 O1 C1 C2 -52.86(16) . . . . ?
 Fe1 N1 C2 C1 -9.73(17) . . . . ?
 Fe1 N1 C2 C3 -130.76(11) . . . . ?
 Fe1 N1 C2 C5 112.98(12) . . . . ?
 Fe1 N1 C4 O2 153.45(10) . . . . ?
 Fe1 N1 C4 C7 34.04(15) . . . . ?
 Fe1 N1 C6 O3 -140.84(11) . . . . ?
 Fe1 N1 C6 C12 -20.65(16) . . . . ?
 Fe1 N2 C7 C4 -0.52(19) . . . . ?
 Fe1 N2 C7 C8 178.09(13) . . . . ?
 Fe1 N2 C11 C10 -177.72(14) . . . . ?
 Fe1 N3 C12 C6 -14.1(2) . . . . ?
 Fe1 N3 C12 C13 168.84(13) . . . . ?
 Fe1 N3 C16 C15 -170.62(15) . . . . ?
 O1 C1 C2 N1 38.33(18) . . . . ?
 O1 C1 C2 C3 153.77(14) . . . . ?
 O1 C1 C2 C5 -77.04(17) . . . . ?
 O2 C4 C7 N2 -140.80(15) . . . . ?
 O2 C4 C7 C8 40.6(2) . . . . ?
 O3 C6 C12 N3 141.49(15) . . . . ?
 O3 C6 C12 C13 -41.4(2) . . . . ?
 N1 C2 C3 O2 -11.82(17) . . . . ?
 N1 C2 C5 O3 31.83(16) . . . . ?
 N1 C4 C7 N2 -23.5(2) . . . . ?
 N1 C4 C7 C8 157.84(15) . . . . ?
 N1 C6 C12 N3 23.4(2) . . . . ?
 N1 C6 C12 C13 -159.42(16) . . . . ?
 N2 C7 C8 C9 -0.7(3) . . . . ?
 N3 C12 C13 C14 2.5(3) . . . . ?
 C1 C2 C3 O2 -131.74(14) . . . . ?
 C1 C2 C5 O3 152.10(14) . . . . ?
 C2 N1 C4 O2 32.54(16) . . . . ?
 C2 N1 C4 C7 -86.87(15) . . . . ?
 C2 N1 C6 O3 -18.74(17) . . . . ?
 C2 N1 C6 C12 101.44(15) . . . . ?
 C3 O2 C4 N1 -41.04(16) . . . . ?
 C3 O2 C4 C7 78.44(16) . . . . ?
 C3 C2 C5 O3 -78.27(16) . . . . ?
 C4 O2 C3 C2 31.98(16) . . . . ?
 C4 N1 C2 C1 109.06(15) . . . . ?
 C4 N1 C2 C3 -11.96(16) . . . . ?
 C4 N1 C2 C5 -128.22(14) . . . . ?
 C4 N1 C6 O3 94.51(16) . . . . ?
 C4 N1 C6 C12 -145.31(14) . . . . ?
 C4 C7 C8 C9 177.91(16) . . . . ?
 C5 O3 C6 N1 39.91(17) . . . . ?
 C5 O3 C6 C12 -80.66(16) . . . . ?
 C5 C2 C3 O2 97.63(16) . . . . ?
 C6 O3 C5 C2 -44.41(16) . . . . ?
 C6 N1 C2 C1 -130.77(15) . . . . ?
 C6 N1 C2 C3 108.21(14) . . . . ?
 C6 N1 C2 C5 -8.05(16) . . . . ?
 C6 N1 C4 O2 -81.09(16) . . . . ?
 C6 N1 C4 C7 159.50(13) . . . . ?
 C6 C12 C13 C14 -174.51(17) . . . . ?
 C7 N2 C11 C10 0.2(3) . . . . ?
 C7 C8 C9 C10 1.1(3) . . . . ?
 C8 C9 C10 C11 -0.9(3) . . . . ?
 C9 C10 C11 N2 0.2(3) . . . . ?
 C11 N2 C7 C4 -178.61(15) . . . . ?
 C11 N2 C7 C8 0.0(2) . . . . ?
 C12 N3 C16 C15 1.5(3) . . . . ?
 C12 C13 C14 C15 0.8(3) . . . . ?
 C13 C14 C15 C16 -2.8(3) . . . . ?
 C14 C15 C16 N3 1.7(3) . . . . ?
 C16 N3 C12 C6 173.46(15) . . . . ?
 C16 N3 C12 C13 -3.6(3) . . . . ?
 O6 S1 C17 F1 174.5(6) . . . . ?
 O6 S1 C17 F2 -67.2(8) . . . . ?
 O6 S1 C17 F3 50.5(8) . . . . ?
 O6 S1 C17' F1' -173.2(7) . . . . ?
 O6 S1 C17' F2' -51.7(10) . . . . ?
 O6 S1 C17' F3' 70.2(10) . . . . ?
 O7 S1 C17 F1 57.1(6) . . . . ?
 O7 S1 C17 F2 175.4(7) . . . . ?
 O7 S1 C17 F3 -66.9(7) . . . . ?
 O7 S1 C17' F1' 65.3(7) . . . . ?
 O7 S1 C17' F2' -173.3(9) . . . . ?
 O7 S1 C17' F3' -51.3(9) . . . . ?
 O8 S1 C17 F1 -64.1(7) . . . . ?
 O8 S1 C17 F2 54.3(7) . . . . ?
 O8 S1 C17 F3 172.0(6) . . . . ?
 O8 S1 C17' F1' -54.3(8) . . . . ?
 O8 S1 C17' F2' 67.1(9) . . . . ?
 O8 S1 C17' F3' -170.9(9) . . . . ?
 O9 S2 C18 F4 -177.6(5) . . . . ?
 O9 S2 C18 F5 61.5(5) . . . . ?
 O9 S2 C18 F6 -58.1(5) . . . . ?
 O10 S2 C18 F4 -54.9(4) . . . . ?
 O10 S2 C18 F5 -175.8(4) . . . . ?
 O10 S2 C18 F6 64.6(5) . . . . ?
 O11 S2 C18 F4 63.1(3) . . . . ?
 O11 S2 C18 F5 -57.8(3) . . . . ?
 O11 S2 C18 F6 -177.4(3) . . . . ?
 O9' S2 C18' F4' -175.0(6) . . . . ?
 O9' S2 C18' F5' 64.6(7) . . . . ?
 O9' S2 C18' F6' -55.2(6) . . . . ?
 O10' S2 C18' F4' -54.3(5) . . . . ?
 O10' S2 C18' F5' -174.7(4) . . . . ?
 O10' S2 C18' F6' 65.4(4) . . . . ?
 O11' S2 C18' F4' 63.8(3) . . . . ?
 O11' S2 C18' F5' -56.5(3) . . . . ?
 O11' S2 C18' F6' -176.4(2) . . . . ?


_olex2_submission_original_sample_id  jonon101
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.904
_oxdiff_exptl_absorpt_empirical_full_min  0.672
#===END
data_D

_vrf_PLAT341_jonon96
;
PROBLEM: _C Low Bond Precision on  C-C Bonds ............... 0.01415 Ang. 
RESPONSE: The crystals were polycrystalline. Integration as a
non-merohedral twin improved the model marginally. Usefully, the
structure is unambiguous and confirms the expected connectivity.
;

_vrf_PLAT007_jonon96
;
PROBLEM: _G Number of Unrefined Donor-H Atoms .............. 2 
RESPONSE: The donor-H atoms were not located in the difference
Fourier map and were unable to be refined without heavy restraints.
Therefore they were placed in reasonable positions for hydrogen
bonding and given riding models.
;

_vrf_PLAT301_jonon96
;
PROBLEM: _G Main Residue Disorder ..............(Resd  1  ) .. 25% 
RESPONSE: Both triflato ligands were modeled as disordered over
two positions each: S1, 0.890(8):0.110(8) and S2, 0.70(2):0.30(2).
;

_vrf_PLAT302_jonon96
;
PROBLEM: _G Anion/Solvent/Minor-Residue Disorder (Resd  2  ) .. 50% 
         _G Anion/Solvent/Minor-Residue Disorder (Resd  3  ) .. 100%  
         _G Anion/Solvent/Minor-Residue Disorder (Resd  4  ) .. 100% 
RESPONSE: The CF3 portion of triflate anion S3 is modeled as
disordered over two positions (0.65(5):0.35(5)). Triflate anion
S4 is modeled as disordered over two positions (0.734(7):0.266(7)).
;

_vrf_PLAT860_jonon96
;
PROBLEM: _G Number of Least-Squares Restraints ............. 764 
RESPONSE: For the various disordered species, analogous bond lengths
and angles were restrained to be similar. Anisotropic displacement
parameters were restrained to be similar and additionally restrained
toward the expected thermal motion relative to bond direction.
;

_vrf_PLAT870_jonon96
;
PROBLEM: _G ALERTS Related to Twinning Effects Suppressed! 
RESPONSE: The intensity data from the polycrystalline crystal were
integrated as a two-component non-merohedral twin.
;

_vrf_PLAT931_jonon96
;
PROBLEM: _G CIFcalcFCF  Twin Law ( 0 1-1)         Est.d BASF       0.44 
RESPONSE: The intensity data from the polycrystalline crystal were
integrated as a two-component non-merohedral twin. The intensity data
were scaled and reduced according to non-merohedral twin law
[ -1 0 0 / 0.194 0.108 -0.894 / -0193 -1.108 -0.108 ], a 180 degree
rotation around reciprocal lattice [ 0 -0.71 0.71]. There were 7843
unique isolated reflections in the first component, 7746 unique
isolated reflections in the second component, and 3299 unique
overlapping reflections. The mass ratio of components refined to
0.607(2):0.393(2).
;

_audit_creation_date               2021-05-15
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

#CrysAlisPro, version 171.40.84a
Rigaku Oxford Diffraction (2020). CrysAlisPro Software system,
version 171.40.84a. Rigaku Corporation, Oxford, UK.

#SHELXT-2018/2
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3--8.

#SHELXL-2018/3
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3--8.
;
_publ_contact_author_name        'William D. Jones'
_publ_contact_author_address     
;
 'Department of Chemistry, University of Rochester, Rochester, New York 14627'
;
_publ_contact_author_email       'jones@chem.rochester.edu'
_publ_requested_journal          'J. Am. Chem. Soc.'
_publ_section_title            
;
Iron-Based Dehydration Catalyst for Selective Formation of Styrene
;

loop_
_publ_author_name                
 'Olaf Nachtigall'
 'Andrew I. VanderWeide'
 'William W. Brennessel'
 'William D. Jones'

_publ_author_address             
;
 Department of Chemistry, University of Rochester, Rochester, NY  14627 USA
;

_chemical_name_common              jonon96
_chemical_name_systematic          '{[(FOX)Fe(OTf)]2(u-O)}[OTf]2'
_chemical_formula_moiety           'C34 H30 F6 Fe2 N6 O13 S2, 2(C F3 O3 S)'
_chemical_formula_sum              'C36 H30 F12 Fe2 N6 O19 S4'
_chemical_formula_weight           1318.60
_chemical_melting_point            ?
_chemical_oxdiff_formula           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 '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'
 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Fe' 'Fe' -1.1336 3.1974
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system        'triclinic'
_space_group_IT_number             2
_space_group_name_H-M_alt          'P -1'
_space_group_name_Hall             '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                     13.3866(5)
_cell_length_b                     13.6776(9)
_cell_length_c                     14.4554(5)
_cell_angle_alpha                  97.802(4)
_cell_angle_beta                   97.381(3)
_cell_angle_gamma                  106.208(5)
_cell_volume                       2479.2(2)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      9515
_cell_measurement_temperature      100.00(10)
_cell_measurement_theta_max        74.1440
_cell_measurement_theta_min        3.1360
_shelx_estimated_absorpt_T_max     0.736
_shelx_estimated_absorpt_T_min     0.510
_exptl_absorpt_coefficient_mu      7.416
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.70803
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              red
_exptl_crystal_colour_primary      red
_exptl_crystal_density_diffrn      1.766
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1328
_exptl_crystal_size_max            0.105
_exptl_crystal_size_mid            0.059
_exptl_crystal_size_min            0.044
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    ?
_diffrn_reflns_av_unetI/netI       0.0374
_diffrn_reflns_Laue_measured_fraction_full  0.990
_diffrn_reflns_Laue_measured_fraction_max  0.965
_diffrn_reflns_limit_h_max         16
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         17
_diffrn_reflns_limit_k_min         -15
_diffrn_reflns_limit_l_max         16
_diffrn_reflns_limit_l_min         -18
_diffrn_reflns_number              18888
_diffrn_reflns_point_group_measured_fraction_full  0.990
_diffrn_reflns_point_group_measured_fraction_max  0.965
_diffrn_reflns_theta_full          74.504
_diffrn_reflns_theta_max           78.878
_diffrn_reflns_theta_min           3.134
_diffrn_ambient_environment        N~2~
_diffrn_ambient_temperature        100.00(10)
_diffrn_detector                   'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean   10.0000
_diffrn_detector_type              HyPix
_diffrn_measured_fraction_theta_full  0.990
_diffrn_measured_fraction_theta_max  0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -26.00   1.00   0.50    6.14    --  -49.62  75.00-133.00   54
  2  ω    -30.00  22.00   0.50    6.14    --  -49.62  38.00-150.00  104
  3  ω    -61.00 -30.00   0.50   24.57    --  -84.25  75.00-133.00   62
  4  ω    -42.00 -17.00   0.50   24.57    --  -84.25  45.00  30.00   50
  5  ω    -93.00 -31.00   0.50    6.14    --  -49.62 -75.00  98.00  124
  6  ω     31.00 115.00   0.50    6.14    --   49.62  75.00-133.00  168
  7  ω    150.00 177.00   0.50   24.57    --  105.75  75.00-133.00   54
  8  ω    109.00 175.00   0.50   24.57    --  105.75 125.00-150.00  132
  9  ω     97.00 135.00   0.50   24.57    --  105.75  75.00-133.00   76
 10  ω    102.00 161.00   0.50   24.57    --  105.75  15.00 -60.00  118
 11  ω     99.00 175.00   0.50   24.57    --  105.75  45.00  60.00  152
 12  ω    125.00 170.00   0.50   24.57    --  105.75 125.00 150.00   90
 13  ω     99.00 178.00   0.50   24.57    --  105.75  30.00 150.00  158
 14  ω    108.00 177.00   0.50   24.57    --  105.75  30.00 120.00  138
 15  ω     71.00 102.00   0.50   24.57    --  105.75 -75.00  98.00   62
 16  ω     85.00 112.00   0.50   24.57    --  105.75-125.00  30.00   54
 17  ω     86.00 116.00   0.50   24.57    --  105.75-125.00  60.00   60
 18  ω     74.00 131.00   0.50   24.57    --  105.75-144.00  -6.23  114
 19  ω     61.00  87.00   0.50   24.57    --  105.75 -94.00-150.00   52
 20  ω     44.00  78.00   0.50   24.57    --  105.75 -61.00 -90.00   68
 21  ω     34.00 100.00   0.50   24.57    --  105.75 -94.00 -90.00  132
 22  ω     35.00  82.00   0.50   24.57    --  105.75 -61.00 -60.00   94
 23  ω     98.00 158.00   0.50   24.57    --  105.75  15.00-120.00  120
 24  ω     99.00 161.00   0.50   24.57    --  105.75  15.00-150.00  124
 25  ω     51.00 109.00   0.50   24.57    --  105.75 -94.00  60.00  116
 26  ω     53.00  79.00   0.50   24.57    --  105.75 -61.00 150.00   52
 27  ω     46.00  72.00   0.50   24.57    --  105.75 -61.00 120.00   52
 28  ω     46.00 108.00   0.50   24.57    --  105.75 -94.00 120.00  124
 29  ω     39.00  67.00   0.50   24.57    --  105.75-125.00  60.00   56
 30  ω     31.00  94.00   0.50    6.14    --   49.62-125.00  90.00  126
 31  ω     34.00  62.00   0.50   24.57    --  105.75 -61.00 -30.00   56
 32  ω     37.00  87.00   0.50   24.57    --  105.75 -94.00 -60.00  100
 33  ω     38.00  87.00   0.50   24.57    --  105.75 -77.00-150.00   98
 34  ω     48.00 108.00   0.50   24.57    --  105.75 -94.00-180.00  120
 35  ω    -22.00   3.00   0.50    6.14    --   49.62 -19.00   0.00   50
 36  ω    -22.00   3.00   0.50    6.14    --   49.62 -19.00 -30.00   50
 37  ω      3.00  66.00   0.50    6.14    --   49.62 -75.00  98.00  126
 38  ω    -21.00   4.00   0.50    6.14    --   49.62 -19.00  90.00   50
 39  ω    -21.00   4.00   0.50    6.14    --   49.62 -19.00 120.00   50
 40  ω   -101.00 -73.00   0.50    6.14    --  -49.62-125.00  60.00   56
 41  ω   -114.00 -89.00   0.50    6.14    --  -49.62-125.00 120.00   50
 42  ω   -110.00 -85.00   0.50   24.57    --  -84.25 -75.00  98.00   50
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0712269000
_diffrn_orient_matrix_UB_12        -0.0787063000
_diffrn_orient_matrix_UB_13        -0.0860354000
_diffrn_orient_matrix_UB_21        -0.0963871000
_diffrn_orient_matrix_UB_22        0.0312513000
_diffrn_orient_matrix_UB_23        0.0256843000
_diffrn_orient_matrix_UB_31        0.0212951000
_diffrn_orient_matrix_UB_32        0.0840017000
_diffrn_orient_matrix_UB_33        -0.0622456000
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             'Cu K\a'
_diffrn_radiation_wavelength       1.54184
_diffrn_source                     'micro-focus sealed X-ray tube'
_diffrn_source_type                'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  12885
_reflns_number_total               18888
_reflns_odcompleteness_completeness  98.94
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       74.33
_reflns_special_details
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection         'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction          'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics      'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015b)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2015a)'
_refine_diff_density_max           1.181
_refine_diff_density_min           -1.133
_refine_diff_density_rms           0.170
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.287
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       969
_refine_ls_number_reflns           18888
_refine_ls_number_restraints       764
_refine_ls_R_factor_all            0.1483
_refine_ls_R_factor_gt             0.1074
_refine_ls_restrained_S_all        1.281
_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/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.2853
_refine_ls_wR_factor_ref           0.3316
_refine_special_details
;
The intensity data from the polycrystalline crystal were
integrated as a two-component non-merohedral twin. The intensity data
were scaled and reduced according to non-merohedral twin law
[ -1 0 0 / 0.194 0.108 -0.894 / -0193 -1.108 -0.108 ], a 180 degree
rotation around reciprocal lattice [ 0 -0.71 0.71]. There were 7843
unique isolated reflections in the first component, 7746 unique
isolated reflections in the second component, and 3299 unique
overlapping reflections. The mass ratio of components refined to
0.607(2):0.393(2).

Both triflato ligands were modeled as disordered over two positions
each: S1, 0.890(8):0.110(8) and S2, 0.70(2):0.30(2). The CF3 portion
of triflate anion S3 is modeled as disordered over two positions
(0.65(5):0.35(5)). Triflate anion S4 is modeled as disordered over
two positions (0.734(7):0.266(7)).

For the various disordered species, analogous bond lengths and
angles were restrained to be similar. Anisotropic displacement
parameters were restrained to be similar and additionally restrained
toward the expected thermal motion relative to bond direction.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6067(19)
 0.3933(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 Fe1-O8 \\sim Fe1-O8A
 with sigma of 0.01
 O8-S1 \\sim O8A-S1A
 with sigma of 0.01
 S1-O9 \\sim S1-O10 \\sim S1A-O9A \\sim S1A-O10A
 with sigma of 0.01
 O8-O9 \\sim O8-O10 \\sim O8A-O9A \\sim O8A-O10A
 with sigma of 0.02
 O9-O10 \\sim O9A-O10A
 with sigma of 0.02
 S1-C33 \\sim S1A-C33A
 with sigma of 0.01
 C33-F1 \\sim C33-F2 \\sim C33-F3 \\sim C33A-F1A \\sim C33A-F2A \\sim C33A-F3A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.02
 Fe2-O11 \\sim Fe2-O11A
 with sigma of 0.01
 O11-S2 \\sim O11A-S2A
 with sigma of 0.01
 S2-O12 \\sim S2-O13 \\sim S2A-O12A \\sim S2A-O13A
 with sigma of 0.01
 O11-O12 \\sim O11-O13 \\sim O11A-O12A \\sim O11A-O13A
 with sigma of 0.02
 O12-O13 \\sim O12A-O13A
 with sigma of 0.02
 S2-C34 \\sim S2A-C34A
 with sigma of 0.01
 C34-F4 \\sim C34-F5 \\sim C34-F6 \\sim C34A-F4A \\sim C34A-F5A \\sim C34A-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.02
 S3-C35 \\sim S3-C35A
 with sigma of 0.01
 C35-F7 \\sim C35-F8 \\sim C35-F9 \\sim C35A-F7A \\sim C35A-F8A \\sim C35A-F9A
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.02
 S4-O17 \\sim S4-O18 \\sim S4-O19 \\sim S4A-O17A \\sim S4A-O18A \\sim S4A-O19A
 with sigma of 0.01
 O17-O18 \\sim O18-O19 \\sim O19-O17 \\sim O17A-O18A \\sim O18A-O19A \\sim
O19A-O17A
 with sigma of 0.02
 S4-C36 \\sim S4A-C36A
 with sigma of 0.01
 C36-F10 \\sim C36-F11 \\sim C36-F12 \\sim C36A-F10A \\sim C36A-F11A \\sim
C36A-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.2A
O11 \\sim O11A: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
Uanis(O8) \\sim Ueq, Uanis(O8A) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O9A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 S1, F1, F2, F3, O8, O9, O10, C33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, F1A, F2A, F3A, O8A, O9A, O10A, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, F4, F5, F6, O11, O12, O13, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2A, F4A, F5A, F6A, O11A, O12A, O13A, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S3, F7, F8, F9, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S3, F7A, F8A, F9A, C35A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S4, F10, F11, F12, O17, O18, O19, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S4A, F10A, F11A, F12A, O17A, O18A, O19A, C36A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O11A)=Sof(O12A)=Sof(O13A)=Sof(C34A)=1-
 FVAR(1)
 Sof(S2)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(O11)=Sof(O12)=Sof(O13)=Sof(C34)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(C35A)=1-FVAR(2)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(C35)=FVAR(2)
 Sof(S4A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(O17A)=Sof(O18A)=Sof(O19A)=
 Sof(C36A)=1-FVAR(3)
 Sof(S4)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(O17)=Sof(O18)=Sof(O19)=Sof(C36)=FVAR(3)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(C33A)=1-
 FVAR(4)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O8)=Sof(O9)=Sof(O10)=Sof(C33)=FVAR(4)
7.a Riding coordinates:
 O1(H1), O4(H4)
7.b Ternary CH refined with riding coordinates:
 C4(H4A), C6(H6), C20(H20), C22(H22)
7.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C17(H17A,H17B), C19(H19A,H19B)
7.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16),
 C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32)
;
_atom_sites_solution_hydrogens     mixed
_atom_sites_solution_primary       dual
_atom_sites_solution_secondary     difmap
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
 Fe1 Fe 0.30053(9) 0.67343(8) 0.15438(7) 0.0392(3) Uani 1 1 d D . . . .
 Fe2 Fe 0.21659(9) 0.84931(9) 0.30657(8) 0.0416(3) Uani 1 1 d D . . . .
 S1 S 0.56133(19) 0.7998(2) 0.22134(17) 0.0509(7) Uani 0.890(8) 1 d D U P A 1
 F1 F 0.7275(7) 0.9322(6) 0.1821(7) 0.074(2) Uani 0.890(8) 1 d D U P A 1
 F2 F 0.6312(6) 0.8238(7) 0.0628(5) 0.091(3) Uani 0.890(8) 1 d D U P A 1
 F3 F 0.5804(6) 0.9470(6) 0.1210(7) 0.090(2) Uani 0.890(8) 1 d D U P A 1
 O8 O 0.4543(5) 0.7694(6) 0.1647(6) 0.0464(18) Uani 0.890(8) 1 d D U P A 1
 O9 O 0.5730(9) 0.8645(8) 0.3080(5) 0.080(3) Uani 0.890(8) 1 d D U P A 1
 O10 O 0.6069(7) 0.7189(7) 0.2190(9) 0.095(3) Uani 0.890(8) 1 d D U P A 1
 C33 C 0.6292(6) 0.8799(7) 0.1437(6) 0.059(2) Uani 0.890(8) 1 d D . P A 1
 S1A S 0.5465(18) 0.851(2) 0.203(2) 0.102(9) Uani 0.110(8) 1 d D U P A 2
 F1A F 0.740(6) 0.907(4) 0.204(4) 0.071(15) Uani 0.110(8) 1 d D U P A 2
 F2A F 0.667(5) 0.781(5) 0.091(4) 0.120(18) Uani 0.110(8) 1 d D U P A 2
 F3A F 0.691(6) 0.754(5) 0.232(6) 0.135(17) Uani 0.110(8) 1 d D U P A 2
 O8A O 0.4627(14) 0.750(3) 0.183(4) 0.033(10) Uani 0.110(8) 1 d D U P A 2
 O9A O 0.566(8) 0.900(5) 0.297(3) 0.084(17) Uani 0.110(8) 1 d D U P A 2
 O10A O 0.540(6) 0.908(5) 0.131(4) 0.099(16) Uani 0.110(8) 1 d D U P A 2
 C33A C 0.665(3) 0.818(4) 0.180(4) 0.093(14) Uani 0.110(8) 1 d D . P A 2
 O1 O 0.1596(4) 0.5559(4) 0.1028(4) 0.0480(12) Uani 1 1 d . . . . .
 H1 H 0.118885 0.515695 0.132339 0.072 Uiso 1 1 d R U . . .
 O2 O 0.3828(4) 0.4103(4) 0.0453(4) 0.0476(12) Uani 1 1 d . . . . .
 O3 O 0.3723(4) 0.5515(4) -0.1079(4) 0.0475(12) Uani 1 1 d . . . . .
 O4 O 0.3318(4) 0.8829(5) 0.4266(4) 0.0521(13) Uani 1 1 d . . . . .
 H4 H 0.355376 0.843794 0.459148 0.078 Uiso 1 1 d R U . . .
 O5 O 0.0991(5) 0.9716(6) 0.5349(5) 0.0700(19) Uani 1 1 d . . . . .
 O6 O 0.2054(6) 1.1487(5) 0.4245(5) 0.0693(18) Uani 1 1 d . . . . .
 O7 O 0.2563(5) 0.7521(4) 0.2396(4) 0.0491(12) Uani 1 1 d . . . . .
 N1 N 0.1799(5) 0.9709(5) 0.4010(5) 0.0503(15) Uani 1 1 d . . . . .
 N2 N 0.0973(5) 0.7605(5) 0.3685(5) 0.0477(14) Uani 1 1 d . . . . .
 N3 N 0.2964(5) 0.9900(5) 0.2643(5) 0.0494(14) Uani 1 1 d . . . . .
 N4 N 0.3446(4) 0.5664(4) 0.0474(4) 0.0377(12) Uani 1 1 d . . . . .
 N5 N 0.3602(5) 0.5825(5) 0.2381(4) 0.0427(13) Uani 1 1 d . . . . .
 N6 N 0.2832(5) 0.7333(5) 0.0280(4) 0.0437(13) Uani 1 1 d . . . . .
 C1 C 0.1479(6) 0.5008(7) 0.0079(6) 0.0519(18) Uani 1 1 d . . . . .
 H1A H 0.127141 0.540907 -0.037331 0.062 Uiso 1 1 calc R U . . .
 H1B H 0.092622 0.435280 -0.001308 0.062 Uiso 1 1 calc R U . . .
 C2 C 0.2516(6) 0.4811(6) -0.0099(5) 0.0450(16) Uani 1 1 d . . . . .
 C3 C 0.2689(6) 0.3858(6) 0.0250(7) 0.0524(18) Uani 1 1 d . . . . .
 H3A H 0.238563 0.374881 0.081546 0.063 Uiso 1 1 calc R U . . .
 H3B H 0.237978 0.324306 -0.023550 0.063 Uiso 1 1 calc R U . . .
 C4 C 0.4155(5) 0.5140(5) 0.0940(5) 0.0400(15) Uani 1 1 d . . . . .
 H4A H 0.488488 0.547601 0.087343 0.048 Uiso 1 1 calc R U . . .
 C5 C 0.2683(7) 0.4827(7) -0.1130(6) 0.0535(19) Uani 1 1 d . . . . .
 H5A H 0.262654 0.413800 -0.145087 0.064 Uiso 1 1 calc R U . . .
 H5B H 0.215844 0.507361 -0.147296 0.064 Uiso 1 1 calc R U . . .
 C6 C 0.3905(6) 0.6244(6) -0.0239(5) 0.0415(15) Uani 1 1 d . . . . .
 H6 H 0.466589 0.657134 -0.002354 0.050 Uiso 1 1 calc R U . . .
 C7 C 0.4089(6) 0.5184(6) 0.1977(5) 0.0440(16) Uani 1 1 d . . . . .
 C8 C 0.4526(7) 0.4589(7) 0.2497(6) 0.056(2) Uani 1 1 d . . . . .
 H8 H 0.486142 0.415030 0.220944 0.068 Uiso 1 1 calc R U . . .
 C9 C 0.4465(9) 0.4642(9) 0.3450(7) 0.067(2) Uani 1 1 d . . . . .
 H9 H 0.474307 0.423249 0.380678 0.080 Uiso 1 1 calc R U . . .
 C10 C 0.3981(9) 0.5322(9) 0.3859(7) 0.066(2) Uani 1 1 d . . . . .
 H10 H 0.393543 0.537959 0.449998 0.079 Uiso 1 1 calc R U . . .
 C11 C 0.3575(7) 0.5901(7) 0.3318(5) 0.0500(18) Uani 1 1 d . . . . .
 H11 H 0.326650 0.636752 0.360212 0.060 Uiso 1 1 calc R U . . .
 C12 C 0.3358(6) 0.7068(6) -0.0392(5) 0.0443(16) Uani 1 1 d . . . . .
 C13 C 0.3435(7) 0.7526(7) -0.1177(6) 0.0522(18) Uani 1 1 d . . . . .
 H13 H 0.381334 0.733430 -0.162913 0.063 Uiso 1 1 calc R U . . .
 C14 C 0.2948(8) 0.8269(8) -0.1288(6) 0.060(2) Uani 1 1 d . . . . .
 H14 H 0.298582 0.858387 -0.181901 0.072 Uiso 1 1 calc R U . . .
 C15 C 0.2395(8) 0.8549(8) -0.0596(6) 0.061(2) Uani 1 1 d . . . . .
 H15 H 0.206332 0.905563 -0.065761 0.073 Uiso 1 1 calc R U . . .
 C16 C 0.2346(7) 0.8068(7) 0.0174(6) 0.0517(18) Uani 1 1 d . . . . .
 H16 H 0.197237 0.824932 0.063430 0.062 Uiso 1 1 calc R U . . .
 C17 C 0.3608(7) 0.9838(7) 0.4811(6) 0.055(2) Uani 1 1 d . . . . .
 H17A H 0.408872 1.031590 0.451178 0.066 Uiso 1 1 calc R U . . .
 H17B H 0.396997 0.984385 0.543827 0.066 Uiso 1 1 calc R U . . .
 C18 C 0.2626(7) 1.0184(7) 0.4893(6) 0.058(2) Uani 1 1 d . . . . .
 C19 C 0.2063(8) 0.9736(10) 0.5677(7) 0.070(3) Uani 1 1 d . . . . .
 H19A H 0.210919 0.904636 0.571361 0.084 Uiso 1 1 calc R U . . .
 H19B H 0.234993 1.017975 0.629122 0.084 Uiso 1 1 calc R U . . .
 C20 C 0.0798(6) 0.9293(7) 0.4392(6) 0.054(2) Uani 1 1 d . . . . .
 H20 H 0.023195 0.950969 0.406315 0.065 Uiso 1 1 calc R U . . .
 C21 C 0.2838(8) 1.1365(8) 0.4973(7) 0.067(3) Uani 1 1 d . . . . .
 C22 C 0.1797(7) 1.0597(6) 0.3518(6) 0.057(2) Uani 1 1 d . . . . .
 H22 H 0.108943 1.048218 0.315805 0.068 Uiso 1 1 calc R U . . .
 C23 C 0.0473(7) 0.8103(8) 0.4235(6) 0.059(2) Uani 1 1 d . . . . .
 C24 C -0.0348(9) 0.7573(10) 0.4640(8) 0.080(3) Uani 1 1 d . . . . .
 C25 C -0.0681(11) 0.6494(11) 0.4448(10) 0.094(4) Uani 1 1 d . . . . .
 C26 C -0.0161(9) 0.5986(10) 0.3877(9) 0.080(3) Uani 1 1 d . . . . .
 H26 H -0.036835 0.526664 0.373709 0.096 Uiso 1 1 calc R U . . .
 C27 C 0.0672(7) 0.6565(7) 0.3516(7) 0.056(2) Uani 1 1 d . . . . .
 H27 H 0.103594 0.622463 0.314660 0.067 Uiso 1 1 calc R U . . .
 C28 C 0.2581(7) 1.0693(6) 0.2853(6) 0.0546(19) Uani 1 1 d . . . . .
 C29 C 0.2860(9) 1.1567(8) 0.2410(8) 0.070(3) Uani 1 1 d . . . . .
 H29 H 0.259607 1.211971 0.255408 0.084 Uiso 1 1 calc R U . . .
 C30 C 0.3526(10) 1.1584(8) 0.1767(9) 0.078(3) Uani 1 1 d . . . . .
 H30 H 0.370080 1.214642 0.145879 0.093 Uiso 1 1 calc R U . . .
 C31 C 0.3938(8) 1.0787(7) 0.1569(8) 0.069(2) Uani 1 1 d . . . . .
 H31 H 0.439631 1.080065 0.113495 0.082 Uiso 1 1 calc R U . . .
 C32 C 0.3650(7) 0.9955(7) 0.2037(7) 0.058(2) Uani 1 1 d . . . . .
 H32 H 0.394365 0.941796 0.192738 0.070 Uiso 1 1 calc R U . . .
 S2 S -0.0197(4) 0.8210(4) 0.1765(4) 0.0498(12) Uani 0.700(16) 1 d D U P B 1
 F4 F -0.1288(10) 0.8726(15) 0.0379(14) 0.096(6) Uani 0.700(16) 1 d D U P B 1
 F5 F 0.0361(11) 0.9150(13) 0.0318(10) 0.090(4) Uani 0.700(16) 1 d D U P B 1
 F6 F -0.0210(12) 0.9945(8) 0.1398(8) 0.089(4) Uani 0.700(16) 1 d D U P B 1
 O11 O 0.0960(7) 0.8536(10) 0.2032(9) 0.0516(18) Uani 0.700(16) 1 d D U P B 1
 O12 O -0.0709(9) 0.8535(14) 0.2479(7) 0.089(4) Uani 0.700(16) 1 d D U P B 1
 O13 O -0.0613(12) 0.7182(7) 0.1288(10) 0.092(5) Uani 0.700(16) 1 d D U P B 1
 C34 C -0.0333(10) 0.9025(9) 0.0901(8) 0.057(3) Uani 0.700(16) 1 d D U P B 1
 S2A S -0.0043(10) 0.8039(9) 0.1477(10) 0.052(3) Uani 0.300(16) 1 d D U P B 2
 F4A F -0.1258(16) 0.894(3) 0.049(3) 0.064(7) Uani 0.300(16) 1 d D U P B 2
 F5A F 0.030(2) 0.9950(18) 0.109(2) 0.089(8) Uani 0.300(16) 1 d D U P B 2
 F6A F 0.010(3) 0.856(3) 0.011(2) 0.098(10) Uani 0.300(16) 1 d D U P B 2
 O11A O 0.0959(15) 0.864(2) 0.210(2) 0.052(2) Uani 0.300(16) 1 d D U P B 2
 O12A O -0.0883(16) 0.773(2) 0.197(2) 0.078(8) Uani 0.300(16) 1 d D U P B 2
 O13A O 0.006(3) 0.7259(17) 0.0794(17) 0.081(8) Uani 0.300(16) 1 d D . P B 2
 C34A C -0.0279(19) 0.8982(16) 0.0796(17) 0.058(6) Uani 0.300(16) 1 d D U P B
 2
 S3 S 0.38518(19) 0.75622(18) 0.61686(15) 0.0570(5) Uani 1 1 d D . . . .
 O14 O 0.4061(6) 0.7630(6) 0.5224(4) 0.0659(17) Uani 1 1 d . . . . .
 O15 O 0.4534(6) 0.7154(6) 0.6725(5) 0.0745(19) Uani 1 1 d . . . . .
 O16 O 0.3648(8) 0.8452(6) 0.6641(5) 0.080(2) Uani 1 1 d . . . . .
 F7 F 0.227(2) 0.635(2) 0.6745(13) 0.101(7) Uani 0.65(5) 1 d D U P C 1
 F8 F 0.1851(12) 0.705(2) 0.5584(13) 0.097(6) Uani 0.65(5) 1 d D U P C 1
 F9 F 0.2492(16) 0.5797(17) 0.5359(14) 0.091(5) Uani 0.65(5) 1 d D U P C 1
 C35 C 0.2553(13) 0.6637(13) 0.5959(11) 0.077(4) Uani 0.65(5) 1 d D U P C 1
 F7A F 0.233(3) 0.636(3) 0.6840(18) 0.073(8) Uani 0.35(5) 1 d D U P C 2
 F8A F 0.186(3) 0.647(5) 0.542(2) 0.123(11) Uani 0.35(5) 1 d D U P C 2
 F9A F 0.286(4) 0.557(2) 0.571(4) 0.101(12) Uani 0.35(5) 1 d D U P C 2
 C35A C 0.269(2) 0.645(2) 0.603(2) 0.082(8) Uani 0.35(5) 1 d D U P C 2
 S4 S 0.1057(3) 0.3813(2) 0.2644(2) 0.0593(10) Uani 0.734(7) 1 d D U P D 1
 F10 F -0.0844(7) 0.2682(8) 0.2718(7) 0.085(3) Uani 0.734(7) 1 d D U P D 1
 F11 F 0.0395(7) 0.1985(6) 0.3025(6) 0.078(2) Uani 0.734(7) 1 d D . P D 1
 F12 F -0.0153(8) 0.2074(8) 0.1591(7) 0.090(3) Uani 0.734(7) 1 d D U P D 1
 O17 O 0.1924(7) 0.3556(8) 0.2318(7) 0.073(3) Uani 0.734(7) 1 d D . P D 1
 O18 O 0.0565(8) 0.4359(8) 0.2030(7) 0.069(3) Uani 0.734(7) 1 d D U P D 1
 O19 O 0.1183(9) 0.4229(8) 0.3623(6) 0.078(3) Uani 0.734(7) 1 d D . P D 1
 C36 C 0.0054(9) 0.2570(10) 0.2475(6) 0.062(3) Uani 0.734(7) 1 d D U P D 1
 S4A S 0.0196(11) 0.3629(10) 0.2098(11) 0.111(6) Uani 0.266(7) 1 d D U P D 2
 F10A F 0.114(2) 0.281(3) 0.334(3) 0.21(2) Uani 0.266(7) 1 d D . P D 2
 F11A F -0.056(3) 0.207(3) 0.280(3) 0.154(12) Uani 0.266(7) 1 d D U P D 2
 F12A F 0.001(4) 0.367(3) 0.362(3) 0.20(2) Uani 0.266(7) 1 d D . P D 2
 O17A O -0.0755(16) 0.386(2) 0.179(2) 0.102(10) Uani 0.266(7) 1 d D . P D 2
 O18A O 0.1140(19) 0.449(2) 0.228(3) 0.109(12) Uani 0.266(7) 1 d D U P D 2
 O19A O 0.030(3) 0.277(3) 0.146(4) 0.168(16) Uani 0.266(7) 1 d D U P D 2
 C36A C 0.022(2) 0.293(2) 0.306(2) 0.106(8) Uani 0.266(7) 1 d D U P D 2


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
 Fe1 O8 2.084(6) . ?
 Fe1 O8A 2.089(14) . ?
 Fe1 O1 2.079(5) . ?
 Fe1 O7 1.791(5) . ?
 Fe1 N4 2.233(5) . ?
 Fe1 N5 2.089(6) . ?
 Fe1 N6 2.114(6) . ?
 Fe2 O4 2.074(6) . ?
 Fe2 O7 1.779(5) . ?
 Fe2 N1 2.210(6) . ?
 Fe2 N2 2.100(7) . ?
 Fe2 N3 2.135(7) . ?
 Fe2 O11 2.074(7) . ?
 Fe2 O11A 2.072(12) . ?
 S1 O8 1.473(7) . ?
 S1 O9 1.396(7) . ?
 S1 O10 1.403(8) . ?
 S1 C33 1.824(10) . ?
 F1 C33 1.315(9) . ?
 F2 C33 1.317(8) . ?
 F3 C33 1.319(9) . ?
 S1A O8A 1.479(15) . ?
 S1A O9A 1.396(13) . ?
 S1A O10A 1.397(13) . ?
 S1A C33A 1.819(17) . ?
 F1A C33A 1.316(13) . ?
 F2A C33A 1.314(12) . ?
 F3A C33A 1.316(13) . ?
 O1 H1 0.8593 . ?
 O1 C1 1.439(9) . ?
 O2 C3 1.448(9) . ?
 O2 C4 1.416(8) . ?
 O3 C5 1.433(10) . ?
 O3 C6 1.410(8) . ?
 O4 H4 0.8550 . ?
 O4 C17 1.415(10) . ?
 O5 C19 1.443(11) . ?
 O5 C20 1.386(9) . ?
 O6 C21 1.449(11) . ?
 O6 C22 1.425(9) . ?
 N1 C18 1.512(10) . ?
 N1 C20 1.508(11) . ?
 N1 C22 1.489(12) . ?
 N2 C23 1.337(9) . ?
 N2 C27 1.344(11) . ?
 N3 C28 1.339(10) . ?
 N3 C32 1.342(11) . ?
 N4 C2 1.502(9) . ?
 N4 C4 1.489(9) . ?
 N4 C6 1.477(9) . ?
 N5 C7 1.347(8) . ?
 N5 C11 1.351(10) . ?
 N6 C12 1.339(9) . ?
 N6 C16 1.355(10) . ?
 C1 H1A 0.9700 . ?
 C1 H1B 0.9700 . ?
 C1 C2 1.533(10) . ?
 C2 C3 1.525(12) . ?
 C2 C5 1.537(12) . ?
 C3 H3A 0.9700 . ?
 C3 H3B 0.9700 . ?
 C4 H4A 0.9800 . ?
 C4 C7 1.507(10) . ?
 C5 H5A 0.9700 . ?
 C5 H5B 0.9700 . ?
 C6 H6 0.9800 . ?
 C6 C12 1.531(10) . ?
 C7 C8 1.374(11) . ?
 C8 H8 0.9300 . ?
 C8 C9 1.382(13) . ?
 C9 H9 0.9300 . ?
 C9 C10 1.386(12) . ?
 C10 H10 0.9300 . ?
 C10 C11 1.355(13) . ?
 C11 H11 0.9300 . ?
 C12 C13 1.371(11) . ?
 C13 H13 0.9300 . ?
 C13 C14 1.367(12) . ?
 C14 H14 0.9300 . ?
 C14 C15 1.392(12) . ?
 C15 H15 0.9300 . ?
 C15 C16 1.367(12) . ?
 C16 H16 0.9300 . ?
 C17 H17A 0.9700 . ?
 C17 H17B 0.9700 . ?
 C17 C18 1.529(10) . ?
 C18 C19 1.543(15) . ?
 C18 C21 1.547(14) . ?
 C19 H19A 0.9700 . ?
 C19 H19B 0.9700 . ?
 C20 H20 0.9800 . ?
 C20 C23 1.539(14) . ?
 C22 H22 0.9800 . ?
 C22 C28 1.503(13) . ?
 C23 C24 1.384(14) . ?
 C24 C25 1.394(18) . ?
 C25 C26 1.382(16) . ?
 C26 H26 0.9300 . ?
 C26 C27 1.382(13) . ?
 C27 H27 0.9300 . ?
 C28 C29 1.414(15) . ?
 C29 H29 0.9300 . ?
 C29 C30 1.366(17) . ?
 C30 H30 0.9300 . ?
 C30 C31 1.366(15) . ?
 C31 H31 0.9300 . ?
 C31 C32 1.391(14) . ?
 C32 H32 0.9300 . ?
 S2 O11 1.470(9) . ?
 S2 O12 1.400(9) . ?
 S2 O13 1.401(9) . ?
 S2 C34 1.808(11) . ?
 F4 C34 1.321(9) . ?
 F5 C34 1.325(10) . ?
 F6 C34 1.317(9) . ?
 S2A O11A 1.467(12) . ?
 S2A O12A 1.401(11) . ?
 S2A O13A 1.402(12) . ?
 S2A C34A 1.796(14) . ?
 F4A C34A 1.310(11) . ?
 F5A C34A 1.311(11) . ?
 F6A C34A 1.314(11) . ?
 S3 O14 1.439(7) . ?
 S3 O15 1.418(7) . ?
 S3 O16 1.425(7) . ?
 S3 C35 1.802(16) . ?
 S3 C35A 1.813(18) . ?
 F7 C35 1.320(11) . ?
 F8 C35 1.322(11) . ?
 F9 C35 1.318(11) . ?
 F7A C35A 1.329(12) . ?
 F8A C35A 1.330(12) . ?
 F9A C35A 1.327(12) . ?
 S4 O17 1.420(8) . ?
 S4 O18 1.445(8) . ?
 S4 O19 1.422(8) . ?
 S4 C36 1.811(14) . ?
 F10 C36 1.338(10) . ?
 F11 C36 1.329(10) . ?
 F12 C36 1.319(10) . ?
 S4A O17A 1.429(11) . ?
 S4A O18A 1.435(11) . ?
 S4A O19A 1.446(12) . ?
 S4A C36A 1.792(19) . ?
 F10A C36A 1.306(12) . ?
 F11A C36A 1.310(12) . ?
 F12A C36A 1.314(12) . ?

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
 O8 Fe1 N4 85.2(3) . . ?
 O8 Fe1 N5 88.8(3) . . ?
 O8 Fe1 N6 80.4(3) . . ?
 O8A Fe1 N4 83.6(15) . . ?
 O8A Fe1 N6 91.4(15) . . ?
 O1 Fe1 O8 160.9(3) . . ?
 O1 Fe1 O8A 159.2(14) . . ?
 O1 Fe1 N4 76.5(2) . . ?
 O1 Fe1 N5 92.6(2) . . ?
 O1 Fe1 N6 89.6(2) . . ?
 O7 Fe1 O8 98.9(3) . . ?
 O7 Fe1 O8A 100.3(16) . . ?
 O7 Fe1 O1 99.5(2) . . ?
 O7 Fe1 N4 175.9(2) . . ?
 O7 Fe1 N5 101.8(2) . . ?
 O7 Fe1 N6 105.3(2) . . ?
 N5 Fe1 O8A 77.0(13) . . ?
 N5 Fe1 N4 77.7(2) . . ?
 N5 Fe1 N6 152.0(2) . . ?
 N6 Fe1 N4 75.7(2) . . ?
 O4 Fe2 N1 76.3(2) . . ?
 O4 Fe2 N2 94.4(3) . . ?
 O4 Fe2 N3 90.4(3) . . ?
 O4 Fe2 O11 164.3(4) . . ?
 O7 Fe2 O4 98.1(2) . . ?
 O7 Fe2 N1 174.4(3) . . ?
 O7 Fe2 N2 101.9(3) . . ?
 O7 Fe2 N3 104.8(3) . . ?
 O7 Fe2 O11 97.2(5) . . ?
 O7 Fe2 O11A 101.5(10) . . ?
 N2 Fe2 N1 78.6(3) . . ?
 N2 Fe2 N3 151.9(3) . . ?
 N3 Fe2 N1 75.7(3) . . ?
 O11 Fe2 N1 88.5(5) . . ?
 O11 Fe2 N2 86.4(4) . . ?
 O11 Fe2 N3 81.9(4) . . ?
 O11A Fe2 O4 159.9(9) . . ?
 O11A Fe2 N1 84.2(10) . . ?
 O11A Fe2 N2 86.5(8) . . ?
 O11A Fe2 N3 79.9(7) . . ?
 O8 S1 C33 97.5(4) . . ?
 O9 S1 O8 113.7(5) . . ?
 O9 S1 O10 118.5(7) . . ?
 O9 S1 C33 106.9(5) . . ?
 O10 S1 O8 113.5(5) . . ?
 O10 S1 C33 103.5(5) . . ?
 S1 O8 Fe1 143.1(5) . . ?
 F1 C33 S1 112.7(7) . . ?
 F1 C33 F2 107.4(8) . . ?
 F1 C33 F3 107.7(8) . . ?
 F2 C33 S1 111.5(7) . . ?
 F2 C33 F3 105.7(8) . . ?
 F3 C33 S1 111.5(6) . . ?
 O8A S1A C33A 104(2) . . ?
 O9A S1A O8A 113.1(18) . . ?
 O9A S1A O10A 119(2) . . ?
 O9A S1A C33A 107(5) . . ?
 O10A S1A O8A 113.0(18) . . ?
 O10A S1A C33A 97(5) . . ?
 S1A O8A Fe1 146(3) . . ?
 F1A C33A S1A 103(4) . . ?
 F1A C33A F3A 107.5(19) . . ?
 F2A C33A S1A 117(5) . . ?
 F2A C33A F1A 106.9(19) . . ?
 F2A C33A F3A 107.0(19) . . ?
 F3A C33A S1A 114(5) . . ?
 Fe1 O1 H1 130.0 . . ?
 C1 O1 Fe1 116.6(4) . . ?
 C1 O1 H1 107.5 . . ?
 C4 O2 C3 103.0(5) . . ?
 C6 O3 C5 105.3(5) . . ?
 Fe2 O4 H4 131.8 . . ?
 C17 O4 Fe2 117.1(5) . . ?
 C17 O4 H4 109.0 . . ?
 C20 O5 C19 104.3(6) . . ?
 C22 O6 C21 106.5(6) . . ?
 Fe2 O7 Fe1 167.5(3) . . ?
 C18 N1 Fe2 113.5(4) . . ?
 C20 N1 Fe2 112.2(5) . . ?
 C20 N1 C18 103.7(6) . . ?
 C22 N1 Fe2 109.7(5) . . ?
 C22 N1 C18 104.0(7) . . ?
 C22 N1 C20 113.5(6) . . ?
 C23 N2 Fe2 118.0(6) . . ?
 C23 N2 C27 119.6(7) . . ?
 C27 N2 Fe2 122.4(5) . . ?
 C28 N3 Fe2 115.6(6) . . ?
 C28 N3 C32 119.7(8) . . ?
 C32 N3 Fe2 123.3(6) . . ?
 C2 N4 Fe1 113.7(4) . . ?
 C4 N4 Fe1 111.0(4) . . ?
 C4 N4 C2 105.8(5) . . ?
 C6 N4 Fe1 109.1(4) . . ?
 C6 N4 C2 104.0(5) . . ?
 C6 N4 C4 113.2(5) . . ?
 C7 N5 Fe1 118.3(5) . . ?
 C7 N5 C11 118.9(6) . . ?
 C11 N5 Fe1 122.7(5) . . ?
 C12 N6 Fe1 117.0(5) . . ?
 C12 N6 C16 119.0(7) . . ?
 C16 N6 Fe1 123.4(5) . . ?
 O1 C1 H1A 109.5 . . ?
 O1 C1 H1B 109.5 . . ?
 O1 C1 C2 110.8(6) . . ?
 H1A C1 H1B 108.1 . . ?
 C2 C1 H1A 109.5 . . ?
 C2 C1 H1B 109.5 . . ?
 N4 C2 C1 110.5(6) . . ?
 N4 C2 C3 102.0(6) . . ?
 N4 C2 C5 104.1(6) . . ?
 C1 C2 C5 112.8(7) . . ?
 C3 C2 C1 114.2(7) . . ?
 C3 C2 C5 112.2(6) . . ?
 O2 C3 C2 103.6(6) . . ?
 O2 C3 H3A 111.0 . . ?
 O2 C3 H3B 111.0 . . ?
 C2 C3 H3A 111.0 . . ?
 C2 C3 H3B 111.0 . . ?
 H3A C3 H3B 109.0 . . ?
 O2 C4 N4 106.6(5) . . ?
 O2 C4 H4A 109.4 . . ?
 O2 C4 C7 110.8(6) . . ?
 N4 C4 H4A 109.4 . . ?
 N4 C4 C7 111.3(5) . . ?
 C7 C4 H4A 109.4 . . ?
 O3 C5 C2 106.0(6) . . ?
 O3 C5 H5A 110.5 . . ?
 O3 C5 H5B 110.5 . . ?
 C2 C5 H5A 110.5 . . ?
 C2 C5 H5B 110.5 . . ?
 H5A C5 H5B 108.7 . . ?
 O3 C6 N4 106.5(6) . . ?
 O3 C6 H6 110.1 . . ?
 O3 C6 C12 110.9(6) . . ?
 N4 C6 H6 110.1 . . ?
 N4 C6 C12 109.1(5) . . ?
 C12 C6 H6 110.1 . . ?
 N5 C7 C4 118.4(6) . . ?
 N5 C7 C8 121.0(7) . . ?
 C8 C7 C4 120.6(6) . . ?
 C7 C8 H8 120.1 . . ?
 C7 C8 C9 119.9(7) . . ?
 C9 C8 H8 120.1 . . ?
 C8 C9 H9 120.8 . . ?
 C8 C9 C10 118.4(8) . . ?
 C10 C9 H9 120.8 . . ?
 C9 C10 H10 120.3 . . ?
 C11 C10 C9 119.4(8) . . ?
 C11 C10 H10 120.3 . . ?
 N5 C11 C10 122.3(7) . . ?
 N5 C11 H11 118.8 . . ?
 C10 C11 H11 118.8 . . ?
 N6 C12 C6 117.3(6) . . ?
 N6 C12 C13 122.2(7) . . ?
 C13 C12 C6 120.5(6) . . ?
 C12 C13 H13 120.4 . . ?
 C14 C13 C12 119.2(7) . . ?
 C14 C13 H13 120.4 . . ?
 C13 C14 H14 120.4 . . ?
 C13 C14 C15 119.2(8) . . ?
 C15 C14 H14 120.4 . . ?
 C14 C15 H15 120.4 . . ?
 C16 C15 C14 119.2(8) . . ?
 C16 C15 H15 120.4 . . ?
 N6 C16 C15 121.3(7) . . ?
 N6 C16 H16 119.3 . . ?
 C15 C16 H16 119.3 . . ?
 O4 C17 H17A 109.6 . . ?
 O4 C17 H17B 109.6 . . ?
 O4 C17 C18 110.1(7) . . ?
 H17A C17 H17B 108.1 . . ?
 C18 C17 H17A 109.6 . . ?
 C18 C17 H17B 109.6 . . ?
 N1 C18 C17 110.2(6) . . ?
 N1 C18 C19 102.6(7) . . ?
 N1 C18 C21 105.0(7) . . ?
 C17 C18 C19 111.2(8) . . ?
 C17 C18 C21 113.5(8) . . ?
 C19 C18 C21 113.5(7) . . ?
 O5 C19 C18 101.3(8) . . ?
 O5 C19 H19A 111.5 . . ?
 O5 C19 H19B 111.5 . . ?
 C18 C19 H19A 111.5 . . ?
 C18 C19 H19B 111.5 . . ?
 H19A C19 H19B 109.3 . . ?
 O5 C20 N1 107.5(7) . . ?
 O5 C20 H20 109.3 . . ?
 O5 C20 C23 111.2(8) . . ?
 N1 C20 H20 109.3 . . ?
 N1 C20 C23 110.2(6) . . ?
 C23 C20 H20 109.3 . . ?
 O6 C21 C18 105.3(7) . . ?
 O6 C22 N1 106.1(7) . . ?
 O6 C22 H22 109.5 . . ?
 O6 C22 C28 112.5(8) . . ?
 N1 C22 H22 109.5 . . ?
 N1 C22 C28 109.6(6) . . ?
 C28 C22 H22 109.5 . . ?
 N2 C23 C20 119.0(8) . . ?
 N2 C23 C24 121.5(9) . . ?
 C24 C23 C20 119.4(7) . . ?
 C23 C24 C25 119.1(9) . . ?
 C26 C25 C24 118.9(10) . . ?
 C25 C26 H26 120.5 . . ?
 C27 C26 C25 118.9(11) . . ?
 C27 C26 H26 120.5 . . ?
 N2 C27 C26 121.9(8) . . ?
 N2 C27 H27 119.0 . . ?
 C26 C27 H27 119.0 . . ?
 N3 C28 C22 118.3(8) . . ?
 N3 C28 C29 120.4(9) . . ?
 C29 C28 C22 121.2(8) . . ?
 C28 C29 H29 120.7 . . ?
 C30 C29 C28 118.7(9) . . ?
 C30 C29 H29 120.7 . . ?
 C29 C30 H30 119.5 . . ?
 C31 C30 C29 121.1(10) . . ?
 C31 C30 H30 119.5 . . ?
 C30 C31 H31 121.1 . . ?
 C30 C31 C32 117.8(10) . . ?
 C32 C31 H31 121.1 . . ?
 N3 C32 C31 122.3(8) . . ?
 N3 C32 H32 118.8 . . ?
 C31 C32 H32 118.8 . . ?
 O11 S2 C34 99.8(6) . . ?
 O12 S2 O11 113.7(8) . . ?
 O12 S2 O13 117.4(10) . . ?
 O12 S2 C34 103.7(7) . . ?
 O13 S2 O11 112.8(8) . . ?
 O13 S2 C34 107.0(7) . . ?
 S2 O11 Fe2 142.2(9) . . ?
 F4 C34 S2 112.6(13) . . ?
 F4 C34 F5 107.7(11) . . ?
 F5 C34 S2 116.7(10) . . ?
 F6 C34 S2 105.5(9) . . ?
 F6 C34 F4 106.6(10) . . ?
 F6 C34 F5 107.1(11) . . ?
 O11A S2A C34A 100.8(12) . . ?
 O12A S2A O11A 113.7(14) . . ?
 O12A S2A O13A 115.0(16) . . ?
 O12A S2A C34A 108.9(15) . . ?
 O13A S2A O11A 113.3(14) . . ?
 O13A S2A C34A 103.4(15) . . ?
 S2A O11A Fe2 142.2(16) . . ?
 F4A C34A S2A 119(3) . . ?
 F4A C34A F5A 109.9(15) . . ?
 F4A C34A F6A 109.4(15) . . ?
 F5A C34A S2A 117.9(18) . . ?
 F5A C34A F6A 109.5(16) . . ?
 F6A C34A S2A 89(2) . . ?
 O14 S3 C35 102.7(6) . . ?
 O14 S3 C35A 105.3(9) . . ?
 O15 S3 O14 114.8(4) . . ?
 O15 S3 O16 115.4(5) . . ?
 O15 S3 C35 106.9(7) . . ?
 O15 S3 C35A 95.9(14) . . ?
 O16 S3 O14 114.2(4) . . ?
 O16 S3 C35 100.5(7) . . ?
 O16 S3 C35A 108.9(11) . . ?
 F7 C35 S3 112.5(16) . . ?
 F7 C35 F8 107.5(13) . . ?
 F8 C35 S3 109.6(12) . . ?
 F9 C35 S3 111.8(12) . . ?
 F9 C35 F7 107.9(12) . . ?
 F9 C35 F8 107.4(12) . . ?
 F7A C35A S3 112(2) . . ?
 F7A C35A F8A 105.1(15) . . ?
 F8A C35A S3 115(2) . . ?
 F9A C35A S3 112.4(18) . . ?
 F9A C35A F7A 106.9(15) . . ?
 F9A C35A F8A 104.6(16) . . ?
 O17 S4 O18 113.5(6) . . ?
 O17 S4 O19 117.7(7) . . ?
 O17 S4 C36 103.3(5) . . ?
 O18 S4 C36 102.2(6) . . ?
 O19 S4 O18 113.2(6) . . ?
 O19 S4 C36 104.7(5) . . ?
 F10 C36 S4 110.9(8) . . ?
 F11 C36 S4 108.8(8) . . ?
 F11 C36 F10 108.2(9) . . ?
 F12 C36 S4 112.3(8) . . ?
 F12 C36 F10 108.6(10) . . ?
 F12 C36 F11 107.9(9) . . ?
 O17A S4A O18A 114.9(14) . . ?
 O17A S4A O19A 111.4(15) . . ?
 O17A S4A C36A 117.8(17) . . ?
 O18A S4A O19A 111.2(15) . . ?
 O18A S4A C36A 108.5(19) . . ?
 O19A S4A C36A 91(3) . . ?
 F10A C36A S4A 114(2) . . ?
 F10A C36A F11A 114.4(16) . . ?
 F10A C36A F12A 113.8(18) . . ?
 F11A C36A S4A 107(2) . . ?
 F11A C36A F12A 115.0(17) . . ?
 F12A C36A S4A 91(3) . . ?

loop_
  _geom_hbond_atom_site_label_D
  _geom_hbond_atom_site_label_H
  _geom_hbond_atom_site_label_A
  _geom_hbond_distance_DH
  _geom_hbond_distance_HA
  _geom_hbond_distance_DA
  _geom_hbond_angle_DHA
  _geom_hbond_site_symmetry_A
  _geom_hbond_publ_flag
 O1 H1 O18 0.86 1.72 2.568(12) 170.6 . yes
 O1 H1 O18A 0.86 1.75 2.50(3) 145.1 . yes
 O4 H4 O14 0.85 1.75 2.602(8) 177.9 . yes

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Fe1 O1 C1 C2 40.3(8) . . . . ?
 Fe1 N4 C2 C1 10.2(8) . . . . ?
 Fe1 N4 C2 C3 -111.6(5) . . . . ?
 Fe1 N4 C2 C5 131.6(5) . . . . ?
 Fe1 N4 C4 O2 140.1(4) . . . . ?
 Fe1 N4 C4 C7 19.1(7) . . . . ?
 Fe1 N4 C6 O3 -153.8(4) . . . . ?
 Fe1 N4 C6 C12 -34.1(6) . . . . ?
 Fe1 N5 C7 C4 -1.3(9) . . . . ?
 Fe1 N5 C7 C8 178.1(7) . . . . ?
 Fe1 N5 C11 C10 -178.8(8) . . . . ?
 Fe1 N6 C12 C6 8.3(9) . . . . ?
 Fe1 N6 C12 C13 -170.1(6) . . . . ?
 Fe1 N6 C16 C15 169.6(7) . . . . ?
 Fe2 O4 C17 C18 41.4(9) . . . . ?
 Fe2 N1 C18 C17 10.7(10) . . . . ?
 Fe2 N1 C18 C19 -107.7(6) . . . . ?
 Fe2 N1 C18 C21 133.3(6) . . . . ?
 Fe2 N1 C20 O5 136.4(6) . . . . ?
 Fe2 N1 C20 C23 15.0(8) . . . . ?
 Fe2 N1 C22 O6 -153.4(5) . . . . ?
 Fe2 N1 C22 C28 -31.7(8) . . . . ?
 Fe2 N2 C23 C20 -0.4(10) . . . . ?
 Fe2 N2 C23 C24 177.6(8) . . . . ?
 Fe2 N2 C27 C26 -175.6(9) . . . . ?
 Fe2 N3 C28 C22 12.0(10) . . . . ?
 Fe2 N3 C28 C29 -164.1(7) . . . . ?
 Fe2 N3 C32 C31 161.8(8) . . . . ?
 O8 Fe1 O7 Fe2 64.5(18) . . . . ?
 O8 S1 C33 F1 170.8(7) . . . . ?
 O8 S1 C33 F2 -68.3(7) . . . . ?
 O8 S1 C33 F3 49.6(7) . . . . ?
 O9 S1 O8 Fe1 -75.2(10) . . . . ?
 O9 S1 C33 F1 53.2(9) . . . . ?
 O9 S1 C33 F2 174.0(8) . . . . ?
 O9 S1 C33 F3 -68.1(9) . . . . ?
 O10 S1 O8 Fe1 64.2(10) . . . . ?
 O10 S1 C33 F1 -72.7(8) . . . . ?
 O10 S1 C33 F2 48.2(8) . . . . ?
 O10 S1 C33 F3 166.0(8) . . . . ?
 C33 S1 O8 Fe1 172.6(8) . . . . ?
 O8A Fe1 O7 Fe2 76(2) . . . . ?
 O8A S1A C33A F1A -175(4) . . . . ?
 O8A S1A C33A F2A 67(4) . . . . ?
 O8A S1A C33A F3A -59(4) . . . . ?
 O9A S1A O8A Fe1 82(8) . . . . ?
 O9A S1A C33A F1A -55(4) . . . . ?
 O9A S1A C33A F2A -173(4) . . . . ?
 O9A S1A C33A F3A 61(4) . . . . ?
 O10A S1A O8A Fe1 -57(8) . . . . ?
 O10A S1A C33A F1A 69(4) . . . . ?
 O10A S1A C33A F2A -49(4) . . . . ?
 O10A S1A C33A F3A -175(4) . . . . ?
 C33A S1A O8A Fe1 -162(6) . . . . ?
 O1 Fe1 O7 Fe2 -110.0(17) . . . . ?
 O1 C1 C2 N4 -30.8(9) . . . . ?
 O1 C1 C2 C3 83.5(8) . . . . ?
 O1 C1 C2 C5 -146.9(7) . . . . ?
 O2 C4 C7 N5 -131.1(7) . . . . ?
 O2 C4 C7 C8 49.5(10) . . . . ?
 O3 C6 C12 N6 135.6(7) . . . . ?
 O3 C6 C12 C13 -46.0(10) . . . . ?
 O4 Fe2 O7 Fe1 -118.5(17) . . . . ?
 O4 C17 C18 N1 -31.7(11) . . . . ?
 O4 C17 C18 C19 81.3(9) . . . . ?
 O4 C17 C18 C21 -149.2(8) . . . . ?
 O5 C20 C23 N2 -129.3(8) . . . . ?
 O5 C20 C23 C24 52.7(11) . . . . ?
 O6 C22 C28 N3 132.0(8) . . . . ?
 O6 C22 C28 C29 -51.9(11) . . . . ?
 N1 C18 C19 O5 -36.1(8) . . . . ?
 N1 C18 C21 O6 7.4(10) . . . . ?
 N1 C20 C23 N2 -10.1(11) . . . . ?
 N1 C20 C23 C24 171.9(9) . . . . ?
 N1 C22 C28 N3 14.2(10) . . . . ?
 N1 C22 C28 C29 -169.8(8) . . . . ?
 N2 Fe2 O7 Fe1 145.2(17) . . . . ?
 N2 C23 C24 C25 -1.8(18) . . . . ?
 N3 Fe2 O7 Fe1 -26.0(18) . . . . ?
 N3 C28 C29 C30 0.1(15) . . . . ?
 N4 C2 C3 O2 -33.2(7) . . . . ?
 N4 C2 C5 O3 9.5(8) . . . . ?
 N4 C4 C7 N5 -12.6(10) . . . . ?
 N4 C4 C7 C8 167.9(8) . . . . ?
 N4 C6 C12 N6 18.6(9) . . . . ?
 N4 C6 C12 C13 -163.0(7) . . . . ?
 N5 Fe1 O7 Fe2 155.2(17) . . . . ?
 N5 C7 C8 C9 0.2(14) . . . . ?
 N6 Fe1 O7 Fe2 -17.9(18) . . . . ?
 N6 C12 C13 C14 -0.9(14) . . . . ?
 C1 C2 C3 O2 -152.3(6) . . . . ?
 C1 C2 C5 O3 129.3(7) . . . . ?
 C2 N4 C4 O2 16.4(7) . . . . ?
 C2 N4 C4 C7 -104.6(7) . . . . ?
 C2 N4 C6 O3 -32.3(7) . . . . ?
 C2 N4 C6 C12 87.5(6) . . . . ?
 C3 O2 C4 N4 -37.8(7) . . . . ?
 C3 O2 C4 C7 83.4(7) . . . . ?
 C3 C2 C5 O3 -100.0(7) . . . . ?
 C4 O2 C3 C2 44.3(7) . . . . ?
 C4 N4 C2 C1 132.2(7) . . . . ?
 C4 N4 C2 C3 10.4(7) . . . . ?
 C4 N4 C2 C5 -106.4(6) . . . . ?
 C4 N4 C6 O3 82.0(7) . . . . ?
 C4 N4 C6 C12 -158.2(6) . . . . ?
 C4 C7 C8 C9 179.6(9) . . . . ?
 C5 O3 C6 N4 39.2(7) . . . . ?
 C5 O3 C6 C12 -79.4(7) . . . . ?
 C5 C2 C3 O2 77.7(8) . . . . ?
 C6 O3 C5 C2 -29.8(8) . . . . ?
 C6 N4 C2 C1 -108.3(7) . . . . ?
 C6 N4 C2 C3 129.9(6) . . . . ?
 C6 N4 C2 C5 13.1(7) . . . . ?
 C6 N4 C4 O2 -96.8(6) . . . . ?
 C6 N4 C4 C7 142.2(6) . . . . ?
 C6 C12 C13 C14 -179.2(8) . . . . ?
 C7 N5 C11 C10 -2.9(13) . . . . ?
 C7 C8 C9 C10 -1.5(16) . . . . ?
 C8 C9 C10 C11 0.7(17) . . . . ?
 C9 C10 C11 N5 1.5(16) . . . . ?
 C11 N5 C7 C4 -177.4(7) . . . . ?
 C11 N5 C7 C8 2.0(12) . . . . ?
 C12 N6 C16 C15 -0.8(13) . . . . ?
 C12 C13 C14 C15 0.6(15) . . . . ?
 C13 C14 C15 C16 -0.4(16) . . . . ?
 C14 C15 C16 N6 0.5(15) . . . . ?
 C16 N6 C12 C6 179.3(7) . . . . ?
 C16 N6 C12 C13 1.0(12) . . . . ?
 C17 C18 C19 O5 -153.9(7) . . . . ?
 C17 C18 C21 O6 127.9(8) . . . . ?
 C18 N1 C20 O5 13.6(8) . . . . ?
 C18 N1 C20 C23 -107.8(7) . . . . ?
 C18 N1 C22 O6 -31.7(8) . . . . ?
 C18 N1 C22 C28 90.0(7) . . . . ?
 C19 O5 C20 N1 -38.0(10) . . . . ?
 C19 O5 C20 C23 82.8(9) . . . . ?
 C19 C18 C21 O6 -103.9(9) . . . . ?
 C20 O5 C19 C18 46.0(10) . . . . ?
 C20 N1 C18 C17 132.7(8) . . . . ?
 C20 N1 C18 C19 14.2(8) . . . . ?
 C20 N1 C18 C21 -104.7(8) . . . . ?
 C20 N1 C22 O6 80.2(8) . . . . ?
 C20 N1 C22 C28 -158.1(6) . . . . ?
 C20 C23 C24 C25 176.1(11) . . . . ?
 C21 O6 C22 N1 37.6(10) . . . . ?
 C21 O6 C22 C28 -82.3(10) . . . . ?
 C21 C18 C19 O5 76.7(9) . . . . ?
 C22 O6 C21 C18 -27.5(10) . . . . ?
 C22 N1 C18 C17 -108.4(8) . . . . ?
 C22 N1 C18 C19 133.1(7) . . . . ?
 C22 N1 C18 C21 14.2(8) . . . . ?
 C22 N1 C20 O5 -98.6(8) . . . . ?
 C22 N1 C20 C23 140.0(7) . . . . ?
 C22 C28 C29 C30 -176.0(9) . . . . ?
 C23 N2 C27 C26 1.7(15) . . . . ?
 C23 C24 C25 C26 2(2) . . . . ?
 C24 C25 C26 C27 0(2) . . . . ?
 C25 C26 C27 N2 -1.8(19) . . . . ?
 C27 N2 C23 C20 -177.8(8) . . . . ?
 C27 N2 C23 C24 0.2(14) . . . . ?
 C28 N3 C32 C31 -3.9(14) . . . . ?
 C28 C29 C30 C31 -1.7(17) . . . . ?
 C29 C30 C31 C32 0.6(17) . . . . ?
 C30 C31 C32 N3 2.2(16) . . . . ?
 C32 N3 C28 C22 178.8(8) . . . . ?
 C32 N3 C28 C29 2.7(13) . . . . ?
 O11 Fe2 O7 Fe1 57.4(18) . . . . ?
 O11 S2 C34 F4 165.3(13) . . . . ?
 O11 S2 C34 F5 39.9(15) . . . . ?
 O11 S2 C34 F6 -78.8(13) . . . . ?
 O12 S2 O11 Fe2 53.9(17) . . . . ?
 O12 S2 C34 F4 -77.2(12) . . . . ?
 O12 S2 C34 F5 157.5(13) . . . . ?
 O12 S2 C34 F6 38.7(12) . . . . ?
 O13 S2 O11 Fe2 -83.1(18) . . . . ?
 O13 S2 C34 F4 47.6(13) . . . . ?
 O13 S2 C34 F5 -77.7(14) . . . . ?
 O13 S2 C34 F6 163.5(12) . . . . ?
 C34 S2 O11 Fe2 163.7(14) . . . . ?
 O11A Fe2 O7 Fe1 56.4(19) . . . . ?
 O11A S2A C34A F4A -149(2) . . . . ?
 O11A S2A C34A F5A -13(3) . . . . ?
 O11A S2A C34A F6A 99(2) . . . . ?
 O12A S2A O11A Fe2 73(4) . . . . ?
 O12A S2A C34A F4A -29(2) . . . . ?
 O12A S2A C34A F5A 107(2) . . . . ?
 O12A S2A C34A F6A -141(2) . . . . ?
 O13A S2A O11A Fe2 -60(4) . . . . ?
 O13A S2A C34A F4A 93(2) . . . . ?
 O13A S2A C34A F5A -130(2) . . . . ?
 O13A S2A C34A F6A -18(2) . . . . ?
 C34A S2A O11A Fe2 -170(3) . . . . ?
 O14 S3 C35 F7 171.1(12) . . . . ?
 O14 S3 C35 F8 -69.4(11) . . . . ?
 O14 S3 C35 F9 49.5(13) . . . . ?
 O14 S3 C35A F7A -174(2) . . . . ?
 O14 S3 C35A F8A -54(2) . . . . ?
 O14 S3 C35A F9A 66(2) . . . . ?
 O15 S3 C35 F7 49.9(14) . . . . ?
 O15 S3 C35 F8 169.4(11) . . . . ?
 O15 S3 C35 F9 -71.7(14) . . . . ?
 O15 S3 C35A F7A 69(2) . . . . ?
 O15 S3 C35A F8A -171(2) . . . . ?
 O15 S3 C35A F9A -52(2) . . . . ?
 O16 S3 C35 F7 -70.9(13) . . . . ?
 O16 S3 C35 F8 48.6(12) . . . . ?
 O16 S3 C35 F9 167.5(13) . . . . ?
 O16 S3 C35A F7A -51(2) . . . . ?
 O16 S3 C35A F8A 69(2) . . . . ?
 O16 S3 C35A F9A -171(2) . . . . ?
 O17 S4 C36 F10 -177.6(8) . . . . ?
 O17 S4 C36 F11 63.5(8) . . . . ?
 O17 S4 C36 F12 -55.9(8) . . . . ?
 O18 S4 C36 F10 -59.5(8) . . . . ?
 O18 S4 C36 F11 -178.5(7) . . . . ?
 O18 S4 C36 F12 62.1(8) . . . . ?
 O19 S4 C36 F10 58.7(9) . . . . ?
 O19 S4 C36 F11 -60.3(8) . . . . ?
 O19 S4 C36 F12 -179.6(8) . . . . ?
 O17A S4A C36A F10A -176(3) . . . . ?
 O17A S4A C36A F11A 57(3) . . . . ?
 O17A S4A C36A F12A -59(3) . . . . ?
 O18A S4A C36A F10A -43(3) . . . . ?
 O18A S4A C36A F11A -170(3) . . . . ?
 O18A S4A C36A F12A 74(3) . . . . ?
 O19A S4A C36A F10A 70(3) . . . . ?
 O19A S4A C36A F11A -57(2) . . . . ?
 O19A S4A C36A F12A -174(3) . . . . ?


_olex2_submission_original_sample_id  jonon96
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  3.773
_oxdiff_exptl_absorpt_empirical_full_min  0.294
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.6067(19)
 2 0.3933(19)
#===end

