# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_150K
_database_code_depnum_ccdc_archive 'CCDC 2389231'
loop_
_audit_author_name
_audit_author_address
'Leokadiya Zorina'
;Osipyan Insitute of solid State Physics RAS
Russia
;
_audit_update_record             
;
2024-10-07 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H11 Fe N6 O4 S2, H2 O'
_chemical_formula_sum            'C8 H13 Fe N6 O5 S2'
_chemical_formula_weight         393.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.1829(3)
_cell_length_b                   10.4546(3)
_cell_length_c                   12.7936(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.816(3)
_cell_angle_gamma                90
_cell_volume                     1458.47(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    7665
_cell_measurement_theta_min      2.1680
_cell_measurement_theta_max      32.8330

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_F_000             804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.353
_shelx_estimated_absorpt_T_min   0.534
_shelx_estimated_absorpt_T_max   0.728
_exptl_absorpt_correction_T_min  0.85296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      150(1)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_reflns_number            33763
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.191
_diffrn_reflns_theta_max         33.080
_diffrn_reflns_theta_full        32.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             5244
_reflns_number_gt                4680
_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       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_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)+(0.0288P)²+1.0818P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5244
_refine_ls_number_parameters     220
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0256
_refine_ls_wR_factor_ref         0.0636
_refine_ls_wR_factor_gt          0.0607
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
Fe1 Fe 0.07316(2) 0.48030(2) 0.24589(2) 0.01017(4) Uani 1 1 d . . . . .
S1 S 0.18833(3) 0.40292(3) 0.39723(2) 0.01400(6) Uani 1 1 d . . . . .
S2 S 0.22657(3) 0.59181(3) 0.20401(2) 0.01656(6) Uani 1 1 d . . . . .
O1 O -0.04378(8) 0.56553(9) 0.13368(7) 0.01658(16) Uani 1 1 d . . . . .
O2 O -0.05973(8) 0.36209(8) 0.25661(7) 0.01465(15) Uani 1 1 d . . . . .
O3 O -0.17905(8) 0.72449(9) 0.11055(7) 0.01743(17) Uani 1 1 d . . . . .
O4 O -0.12921(9) 0.16799(9) 0.20084(7) 0.01940(18) Uani 1 1 d . . . . .
C1 C 0.14989(10) 0.52416(10) 0.47851(9) 0.01199(18) Uani 1 1 d . . . . .
C2 C -0.05507(10) 0.69081(11) 0.28543(9) 0.01310(19) Uani 1 1 d . . . . .
C3 C -0.09700(10) 0.66042(11) 0.16872(9) 0.01338(19) Uani 1 1 d . . . . .
C4 C 0.25494(10) 0.48563(11) 0.10963(9) 0.01325(19) Uani 1 1 d . . . . .
C5 C 0.02969(10) 0.25780(11) 0.12792(9) 0.01287(19) Uani 1 1 d . . . . .
C6 C -0.06117(10) 0.26071(11) 0.19890(9) 0.01371(19) Uani 1 1 d . . . . .
C7 C -0.10541(12) 0.80021(12) 0.33620(10) 0.0194(2) Uani 1 1 d . . . . .
H7A H -0.125073 0.772044 0.403497 0.029 Uiso 1 1 calc R U . . .
H7B H -0.179959 0.831774 0.287611 0.029 Uiso 1 1 calc R U . . .
H7C H -0.044388 0.868932 0.350954 0.029 Uiso 1 1 calc R U . . .
C8 C 0.02984(12) 0.15109(12) 0.05170(10) 0.0194(2) Uani 1 1 d . . . . .
H8A H -0.029276 0.169171 -0.015532 0.029 Uiso 1 1 calc R U . . .
H8B H 0.006902 0.071551 0.082766 0.029 Uiso 1 1 calc R U . . .
H8C H 0.111990 0.141976 0.037472 0.029 Uiso 1 1 calc R U . . .
N1 N 0.02738(9) 0.61036(9) 0.33427(7) 0.01119(16) Uani 1 1 d . . . . .
N2 N 0.07513(9) 0.62150(9) 0.44210(7) 0.01292(17) Uani 1 1 d . . . . .
N3 N 0.10263(9) 0.35469(9) 0.14557(7) 0.01113(16) Uani 1 1 d . . . . .
N4 N 0.19352(9) 0.37326(9) 0.09093(8) 0.01288(17) Uani 1 1 d D . . . .
H4 H 0.2094(3) 0.3208(8) 0.0503(7) 0.015 Uiso 1 1 calc DR U . . .
N5 N 0.19869(10) 0.51779(10) 0.58320(8) 0.01561(18) Uani 1 1 d D . . . .
H5A H 0.1803(16) 0.5732(15) 0.6235(13) 0.019 Uiso 1 1 d D U . . .
H5B H 0.2493(14) 0.4607(15) 0.6087(13) 0.019 Uiso 1 1 d D U . . .
N6 N 0.33729(10) 0.51040(11) 0.05381(9) 0.01802(19) Uani 1 1 d D . . . .
H6A H 0.3563(17) 0.4577(15) 0.0113(13) 0.022 Uiso 1 1 d D U . . .
H6B H 0.3816(15) 0.5753(14) 0.0678(14) 0.022 Uiso 1 1 d D U . . .
O5W O 0.05691(9) 0.84554(9) 0.57132(7) 0.01669(16) Uani 1 1 d D . . . .
H5W1 H 0.0601(18) 0.7808(16) 0.5438(14) 0.025 Uiso 1 1 d D U . . .
H5W2 H 0.0926(17) 0.8347(18) 0.6285(13) 0.025 Uiso 1 1 d D 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 N1 1.9096(9) . ?
Fe1 N3 1.9152(9) . ?
Fe1 O1 1.9318(8) . ?
Fe1 O2 1.9608(9) . ?
Fe1 S1 2.2262(3) . ?
Fe1 S2 2.2354(3) . ?
S1 C1 1.7523(11) . ?
S2 C4 1.7207(12) . ?
O1 C3 1.2874(14) . ?
O2 C6 1.2897(14) . ?
O3 C3 1.2416(14) . ?
O4 C6 1.2359(14) . ?
C1 N5 1.3312(14) . ?
C1 N2 1.3338(14) . ?
C2 N1 1.3010(14) . ?
C2 C7 1.4862(16) . ?
C2 C3 1.4965(15) . ?
C4 N6 1.3102(15) . ?
C4 N4 1.3551(15) . ?
C5 N3 1.2887(14) . ?
C5 C8 1.4819(16) . ?
C5 C6 1.5058(16) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N1 N2 1.3693(12) . ?
N3 N4 1.3691(13) . ?
N4 H4 0.802(13) . ?
N5 H5A 0.831(13) . ?
N5 H5B 0.837(13) . ?
N6 H6A 0.834(13) . ?
N6 H6B 0.835(13) . ?
O5W H5W1 0.767(15) . ?
O5W H5W2 0.760(15) . ?

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
N1 Fe1 N3 173.55(4) . . ?
N1 Fe1 O1 83.42(4) . . ?
N3 Fe1 O1 90.40(4) . . ?
N1 Fe1 O2 95.77(4) . . ?
N3 Fe1 O2 81.98(4) . . ?
O1 Fe1 O2 86.80(4) . . ?
N1 Fe1 S1 85.59(3) . . ?
N3 Fe1 S1 100.45(3) . . ?
O1 Fe1 S1 168.40(3) . . ?
O2 Fe1 S1 90.65(3) . . ?
N1 Fe1 S2 95.24(3) . . ?
N3 Fe1 S2 86.66(3) . . ?
O1 Fe1 S2 90.59(3) . . ?
O2 Fe1 S2 168.32(3) . . ?
S1 Fe1 S2 94.083(13) . . ?
C1 S1 Fe1 94.74(4) . . ?
C4 S2 Fe1 95.89(4) . . ?
C3 O1 Fe1 112.69(7) . . ?
C6 O2 Fe1 113.03(7) . . ?
N5 C1 N2 118.35(10) . . ?
N5 C1 S1 117.46(9) . . ?
N2 C1 S1 124.19(8) . . ?
N1 C2 C7 125.76(10) . . ?
N1 C2 C3 111.95(10) . . ?
C7 C2 C3 122.29(10) . . ?
O3 C3 O1 122.97(10) . . ?
O3 C3 C2 120.65(10) . . ?
O1 C3 C2 116.38(10) . . ?
N6 C4 N4 117.72(10) . . ?
N6 C4 S2 121.08(9) . . ?
N4 C4 S2 121.19(9) . . ?
N3 C5 C8 127.88(11) . . ?
N3 C5 C6 111.35(10) . . ?
C8 C5 C6 120.76(10) . . ?
O4 C6 O2 124.24(11) . . ?
O4 C6 C5 119.80(10) . . ?
O2 C6 C5 115.94(10) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 N1 N2 120.36(9) . . ?
C2 N1 Fe1 115.50(7) . . ?
N2 N1 Fe1 124.15(7) . . ?
C1 N2 N1 111.17(9) . . ?
C5 N3 N4 122.33(9) . . ?
C5 N3 Fe1 117.39(8) . . ?
N4 N3 Fe1 120.17(7) . . ?
C4 N4 N3 115.94(9) . . ?
C4 N4 H4 122.0 . . ?
N3 N4 H4 122.0 . . ?
C1 N5 H5A 119.1(12) . . ?
C1 N5 H5B 121.2(12) . . ?
H5A N5 H5B 119.6(17) . . ?
C4 N6 H6A 122.5(13) . . ?
C4 N6 H6B 119.9(12) . . ?
H6A N6 H6B 116.8(17) . . ?
H5W1 O5W H5W2 104.1(19) . . ?

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
C8 H8C O3 0.98 2.59 3.2128(16) 121.2 3_565
N4 H4 O3 0.80 2.07 2.7441(13) 142.3 3_565
N5 H5A O2 0.831(13) 2.355(14) 3.0991(14) 149.4(16) 3_566
N5 H5B O4 0.837(13) 2.082(13) 2.9080(13) 168.8(16) 4_666
N6 H6A O5W 0.834(13) 1.972(14) 2.7882(14) 165.7(18) 2_545
N6 H6B O5W 0.835(13) 2.120(15) 2.8472(14) 145.4(17) 4_675
O5W H5W1 N2 0.767(15) 2.143(15) 2.9000(13) 169.2(19) .
O5W H5W2 O4 0.760(15) 2.131(16) 2.8504(13) 158.3(19) 3_566

_refine_diff_density_max         0.654
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.072



####################################################################### 
# 
# 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_350K
_database_code_depnum_ccdc_archive 'CCDC 2389232'
loop_
_audit_author_name
_audit_author_address
'Leokadiya Zorina'
;Osipyan Insitute of solid State Physics RAS
Russia
;
_audit_update_record             
;
2024-10-07 deposited with the CCDC.	2024-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H11 Fe N6 O4 S2, H2 O'
_chemical_formula_sum            'C8 H13 Fe N6 O5 S2'
_chemical_formula_weight         393.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.2865(2)
_cell_length_b                   10.4627(2)
_cell_length_c                   12.9417(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.9640(18)
_cell_angle_gamma                90
_cell_volume                     1489.30(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(1)
_cell_measurement_reflns_used    14669
_cell_measurement_theta_min      2.5130
_cell_measurement_theta_max      32.6670

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_F_000             804
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_exptl_absorpt_coefficient_mu    1.325
_shelx_estimated_absorpt_T_min   0.540
_shelx_estimated_absorpt_T_max   0.733
_exptl_absorpt_correction_T_min  0.87242
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.67a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      350(1)
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            AtlasS2
_diffrn_detector_area_resol_mean 10.4566
_diffrn_reflns_number            34128
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.167
_diffrn_reflns_theta_max         32.980
_diffrn_reflns_theta_full        32.000
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             5271
_reflns_number_gt                4229
_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       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_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)+(0.0395P)²+0.7363P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5271
_refine_ls_number_parameters     220
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0848
_refine_ls_wR_factor_gt          0.0778
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.000
_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
Fe1 Fe 0.07210(2) 0.47865(2) 0.24548(2) 0.02398(6) Uani 1 1 d . . . . .
S1 S 0.18649(4) 0.40289(4) 0.39614(3) 0.03311(10) Uani 1 1 d . . . . .
S2 S 0.22482(5) 0.59011(4) 0.20323(4) 0.03900(11) Uani 1 1 d . . . . .
O1 O -0.04467(12) 0.56378(12) 0.13478(9) 0.0373(3) Uani 1 1 d . . . . .
O2 O -0.05859(11) 0.35885(12) 0.25583(9) 0.0346(3) Uani 1 1 d . . . . .
O3 O -0.17731(12) 0.72269(13) 0.11132(10) 0.0408(3) Uani 1 1 d . . . . .
O4 O -0.12798(13) 0.16625(14) 0.19855(11) 0.0480(3) Uani 1 1 d . . . . .
C1 C 0.14942(14) 0.52525(15) 0.47581(12) 0.0269(3) Uani 1 1 d . . . . .
C2 C -0.05372(15) 0.69058(16) 0.28403(12) 0.0298(3) Uani 1 1 d . . . . .
C3 C -0.09661(15) 0.65910(16) 0.16899(12) 0.0302(3) Uani 1 1 d . . . . .
C4 C 0.25164(15) 0.48492(16) 0.10926(12) 0.0299(3) Uani 1 1 d . . . . .
C5 C 0.02920(14) 0.25710(15) 0.12720(12) 0.0286(3) Uani 1 1 d . . . . .
C6 C -0.06046(15) 0.25903(17) 0.19794(13) 0.0319(3) Uani 1 1 d . . . . .
C7 C -0.1023(2) 0.8020(2) 0.33230(16) 0.0475(5) Uani 1 1 d . . . . .
H7A H -0.121779 0.776526 0.397817 0.071 Uiso 1 1 calc R U . . .
H7B H -0.174346 0.832888 0.284570 0.071 Uiso 1 1 calc R U . . .
H7C H -0.042294 0.868545 0.345723 0.071 Uiso 1 1 calc R U . . .
C8 C 0.0288(2) 0.15145(19) 0.05102(17) 0.0456(5) Uani 1 1 d . . . . .
H8A H -0.027050 0.171098 -0.014675 0.068 Uiso 1 1 calc R U . . .
H8B H 0.004087 0.073757 0.079622 0.068 Uiso 1 1 calc R U . . .
H8C H 0.108972 0.140978 0.038708 0.068 Uiso 1 1 calc R U . . .
N1 N 0.02726(12) 0.61040(12) 0.33275(10) 0.0255(2) Uani 1 1 d . . . . .
N2 N 0.07576(13) 0.62244(13) 0.43945(10) 0.0293(3) Uani 1 1 d . . . . .
N3 N 0.10133(11) 0.35353(12) 0.14506(10) 0.0248(2) Uani 1 1 d . . . . .
N4 N 0.19062(12) 0.37340(13) 0.09042(10) 0.0288(3) Uani 1 1 d D . . . .
H4 H 0.2053(3) 0.3230(10) 0.0507(8) 0.035 Uiso 1 1 calc DR U . . .
N5 N 0.19856(16) 0.52008(15) 0.57908(12) 0.0371(3) Uani 1 1 d D . . . .
H5A H 0.179(2) 0.5738(18) 0.6171(16) 0.045 Uiso 1 1 d D U . . .
H5B H 0.2471(18) 0.4640(19) 0.6023(17) 0.045 Uiso 1 1 d D U . . .
N6 N 0.33270(16) 0.51031(18) 0.05376(14) 0.0436(4) Uani 1 1 d D . . . .
H6A H 0.353(2) 0.456(2) 0.0153(18) 0.052 Uiso 1 1 d D U . . .
H6B H 0.372(2) 0.5768(18) 0.0634(19) 0.052 Uiso 1 1 d D U . . .
O5W O 0.05686(14) 0.84838(14) 0.57196(11) 0.0417(3) Uani 1 1 d D . . . .
H5W1 H 0.059(2) 0.779(2) 0.546(2) 0.063 Uiso 1 1 d D U . . .
H5W2 H 0.099(2) 0.842(3) 0.6297(17) 0.063 Uiso 1 1 d D 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 N1 1.9205(12) . ?
Fe1 N3 1.9246(12) . ?
Fe1 O1 1.9328(12) . ?
Fe1 O2 1.9629(12) . ?
Fe1 S1 2.2288(5) . ?
Fe1 S2 2.2480(5) . ?
S1 C1 1.7524(16) . ?
S2 C4 1.7166(17) . ?
O1 C3 1.285(2) . ?
O2 C6 1.283(2) . ?
O3 C3 1.235(2) . ?
O4 C6 1.235(2) . ?
C1 N2 1.331(2) . ?
C1 N5 1.328(2) . ?
C2 N1 1.295(2) . ?
C2 C7 1.484(2) . ?
C2 C3 1.495(2) . ?
C4 N6 1.311(2) . ?
C4 N4 1.349(2) . ?
C5 N3 1.284(2) . ?
C5 C8 1.480(2) . ?
C5 C6 1.509(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
N1 N2 1.3722(17) . ?
N3 N4 1.3706(18) . ?
N4 H4 0.780(15) . ?
N5 H5A 0.810(15) . ?
N5 H5B 0.813(15) . ?
N6 H6A 0.820(15) . ?
N6 H6B 0.821(15) . ?
O5W H5W1 0.804(19) . ?
O5W H5W2 0.79(2) . ?

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
N1 Fe1 N3 173.24(5) . . ?
N1 Fe1 O1 83.07(5) . . ?
N3 Fe1 O1 90.26(5) . . ?
N1 Fe1 O2 96.72(5) . . ?
N3 Fe1 O2 81.78(5) . . ?
O1 Fe1 O2 86.96(6) . . ?
N1 Fe1 S1 85.31(4) . . ?
N3 Fe1 S1 101.27(4) . . ?
O1 Fe1 S1 167.74(4) . . ?
O2 Fe1 S1 90.57(4) . . ?
N1 Fe1 S2 95.07(4) . . ?
N3 Fe1 S2 86.08(4) . . ?
O1 Fe1 S2 90.75(4) . . ?
O2 Fe1 S2 167.63(4) . . ?
S1 Fe1 S2 94.129(19) . . ?
C1 S1 Fe1 94.99(5) . . ?
C4 S2 Fe1 96.11(6) . . ?
C3 O1 Fe1 112.97(10) . . ?
C6 O2 Fe1 113.22(10) . . ?
N2 C1 N5 118.27(14) . . ?
N2 C1 S1 124.25(12) . . ?
N5 C1 S1 117.48(12) . . ?
N1 C2 C7 126.20(14) . . ?
N1 C2 C3 112.18(13) . . ?
C7 C2 C3 121.62(14) . . ?
O3 C3 O1 122.81(15) . . ?
O3 C3 C2 120.89(15) . . ?
O1 C3 C2 116.31(14) . . ?
N6 C4 N4 117.84(15) . . ?
N6 C4 S2 120.93(14) . . ?
N4 C4 S2 121.24(12) . . ?
N3 C5 C8 127.85(15) . . ?
N3 C5 C6 111.37(13) . . ?
C8 C5 C6 120.76(14) . . ?
O4 C6 O2 124.44(16) . . ?
O4 C6 C5 119.46(15) . . ?
O2 C6 C5 116.09(14) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 N1 N2 120.60(13) . . ?
C2 N1 Fe1 115.39(10) . . ?
N2 N1 Fe1 124.01(10) . . ?
C1 N2 N1 111.24(12) . . ?
C5 N3 N4 122.41(13) . . ?
C5 N3 Fe1 117.26(10) . . ?
N4 N3 Fe1 120.17(10) . . ?
C4 N4 N3 116.27(13) . . ?
C4 N4 H4 121.9 . . ?
N3 N4 H4 121.9 . . ?
C1 N5 H5A 118.3(17) . . ?
C1 N5 H5B 119.7(16) . . ?
H5A N5 H5B 122(2) . . ?
C4 N6 H6A 121.1(18) . . ?
C4 N6 H6B 120.7(17) . . ?
H6A N6 H6B 118(2) . . ?
H5W1 O5W H5W2 105(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
C8 H8C O3 0.96 2.66 3.246(3) 119.9 3_565
N4 H4 O3 0.78 2.10 2.7702(18) 143.6 3_565
N5 H5A O2 0.810(15) 2.460(17) 3.191(2) 151(2) 3_566
N5 H5B O4 0.813(15) 2.147(16) 2.944(2) 167(2) 4_666
N6 H6A O5W 0.820(15) 2.024(17) 2.825(2) 165(2) 2_545
N6 H6B O5W 0.821(15) 2.21(2) 2.894(2) 142(2) 4_675
O5W H5W1 N2 0.804(19) 2.18(2) 2.9562(19) 164(3) .
O5W H5W2 O4 0.79(2) 2.17(2) 2.902(2) 153(3) 3_566

_refine_diff_density_max         0.486
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.072



