# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_as40
_database_code_depnum_ccdc_archive 'CCDC 2218223'
loop_
_audit_author_name
_audit_author_address
'Andrey Utenyshev'
;Federal Research Center of Problems of Chemical Physics and Medicinal Chemistry RAS
Russia
;
_audit_update_record             
;
2023-01-18 deposited with the CCDC.	2023-01-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H6 Cl4 Fe2 N4 O4 S2'
_chemical_formula_weight         587.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0074 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0129 0.0068 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1338 0.1366 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1597 0.1758 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3647 0.9262 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.358(4)
_cell_length_b                   6.4160(13)
_cell_length_c                   17.041(3)
_cell_angle_alpha                90
_cell_angle_beta                 122.66(3)
_cell_angle_gamma                90
_cell_volume                     1966.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    501
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      30.0

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_F_000             1160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    2.560
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.951
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.745
_diffrn_radiation_type           synchrotron
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16024
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.621
_diffrn_reflns_theta_max         31.058
_diffrn_reflns_theta_full        26.551
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2732
_reflns_number_gt                2418
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       mardtb
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    shelxt
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    shelxt
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0568P)²+14.5066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2732
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1387
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_restrained_S_all      1.215
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
Fe Fe 0.53235(3) 0.90444(8) 0.46050(4) 0.01866(15) Uani 1 1 d . . . . .
Cl1 Cl 0.59557(5) 0.35971(15) 0.78135(7) 0.0260(2) Uani 1 1 d . . . . .
S S 0.59124(5) 1.07104(14) 0.59904(6) 0.01965(19) Uani 1 1 d . . . . .
Cl2 Cl 0.75432(5) 0.48612(17) 0.95064(7) 0.0292(2) Uani 1 1 d . . . . .
O1 O 0.57865(18) 0.4841(5) 0.4807(2) 0.0321(7) Uani 1 1 d . . . . .
N1 N 0.55644(18) 0.6509(5) 0.4777(2) 0.0230(6) Uani 1 1 d . . . . .
O2 O 0.5701(2) 1.1021(5) 0.3434(2) 0.0345(7) Uani 1 1 d . . . . .
N2 N 0.55229(18) 1.0370(5) 0.3921(2) 0.0228(6) Uani 1 1 d . . . . .
C4 C 0.7084(2) 0.6417(6) 0.8524(3) 0.0220(7) Uani 1 1 d . . . . .
C3 C 0.6389(2) 0.5821(6) 0.7763(3) 0.0201(6) Uani 1 1 d . . . . .
C2 C 0.6018(2) 0.7059(6) 0.6965(2) 0.0204(7) Uani 1 1 d . . . . .
H2 H 0.556001 0.664831 0.645404 0.024 Uiso 1 1 calc R U . . .
C1 C 0.6345(2) 0.8917(6) 0.6945(2) 0.0198(6) Uani 1 1 d . . . . .
C5 C 0.7408(2) 0.8255(6) 0.8498(3) 0.0234(7) Uani 1 1 d . . . . .
H5 H 0.787182 0.864676 0.900362 0.028 Uiso 1 1 calc R U . . .
C6 C 0.7037(2) 0.9519(6) 0.7710(3) 0.0213(7) Uani 1 1 d . . . . .
H6 H 0.725021 1.076822 0.769230 0.026 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
Fe N2 1.673(3) . ?
Fe N1 1.684(4) . ?
Fe S 2.2567(12) . ?
Fe S 2.2652(12) 5_676 ?
Fe Fe 2.6893(11) 5_676 ?
Cl1 C3 1.728(4) . ?
S C1 1.789(4) . ?
Cl2 C4 1.729(4) . ?
O1 N1 1.160(5) . ?
O2 N2 1.162(4) . ?
C4 C5 1.380(6) . ?
C4 C3 1.397(5) . ?
C3 C2 1.395(5) . ?
C2 C1 1.391(5) . ?
C1 C6 1.398(5) . ?
C5 C6 1.394(5) . ?

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
N2 Fe N1 116.33(16) . . ?
N2 Fe S 106.26(12) . . ?
N1 Fe S 109.29(12) . . ?
N2 Fe S 109.02(12) . 5_676 ?
N1 Fe S 108.54(11) . 5_676 ?
S Fe S 107.01(4) . 5_676 ?
N2 Fe Fe 120.62(12) . 5_676 ?
N1 Fe Fe 123.03(12) . 5_676 ?
S Fe Fe 53.65(3) . 5_676 ?
S Fe Fe 53.36(3) 5_676 5_676 ?
C1 S Fe 111.67(13) . . ?
C1 S Fe 110.90(13) . 5_676 ?
Fe S Fe 72.98(5) . 5_676 ?
O1 N1 Fe 168.0(3) . . ?
O2 N2 Fe 170.1(3) . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 Cl2 119.5(3) . . ?
C3 C4 Cl2 120.2(3) . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 Cl1 118.7(3) . . ?
C4 C3 Cl1 120.6(3) . . ?
C1 C2 C3 118.9(3) . . ?
C2 C1 C6 120.4(3) . . ?
C2 C1 S 123.6(3) . . ?
C6 C1 S 115.9(3) . . ?
C4 C5 C6 119.6(3) . . ?
C5 C6 C1 120.2(4) . . ?

_refine_diff_density_max         0.870
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.142

