# Electronic Supplementary Material (ESI) 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_7a
_database_code_depnum_ccdc_archive 'CCDC 2308698'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2023-11-17 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H17 Fe3 N O6 S2'
_chemical_formula_weight         611.03

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   7.5495(2)
_cell_length_b                   10.6591(3)
_cell_length_c                   28.6528(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2305.72(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7680
_cell_measurement_theta_min      4.3980
_cell_measurement_theta_max      69.4050

_exptl_crystal_description       fragment
_exptl_crystal_colour            red-orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.192
_exptl_crystal_size_rad          0.23
_exptl_absorpt_coefficient_mu    16.973
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_correction_T_min  0.00260
_exptl_absorpt_correction_T_max  0.04575
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Nova (Cu) X-ray Source'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11709
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.085
_diffrn_reflns_theta_max         69.576
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             4194
_reflns_number_gt                4074
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_max     0.930
_reflns_Friedel_fraction_full    0.950

_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 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2022)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_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)+(0.1169P)²] 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_abs_structure_details 
;
 Flack x determined using 1581 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4194
_refine_ls_number_parameters     298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.1551
_refine_ls_wR_factor_gt          0.1542
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_restrained_S_all      1.150
_refine_ls_shift/su_max          0.001
_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
C1 C 0.8143(10) 0.8799(7) 0.4049(2) 0.0519(15) Uani 1 1 d . . . . .
H1A H 0.8235 0.9054 0.4380 0.062 Uiso 1 1 calc R U . . .
H1B H 0.7080 0.8263 0.4017 0.062 Uiso 1 1 calc R U . . .
C2 C 0.9447(11) 0.7382(6) 0.3503(2) 0.0524(15) Uani 1 1 d . . . . .
H2A H 0.8315 0.6916 0.3520 0.063 Uiso 1 1 calc R U . . .
H2B H 1.0415 0.6760 0.3473 0.063 Uiso 1 1 calc R U . . .
C3 C 1.0391(10) 0.7322(7) 0.4322(2) 0.0517(14) Uani 1 1 d . . . . .
H3A H 1.1377 0.6786 0.4212 0.062 Uiso 1 1 calc R U . . .
H3B H 0.9449 0.6772 0.4447 0.062 Uiso 1 1 calc R U . . .
C4 C 1.1035(10) 0.8186(7) 0.4695(2) 0.0499(14) Uani 1 1 d . . . . .
H4 H 1.1973 0.8742 0.4616 0.060 Uiso 1 1 calc R U . . .
C5 C 1.0412(10) 0.8244(6) 0.5124(2) 0.0504(14) Uani 1 1 d . . . . .
H5 H 0.9537 0.7646 0.5209 0.061 Uiso 1 1 calc R U . . .
C6 C 1.0950(9) 0.9150(7) 0.5482(2) 0.0495(14) Uani 1 1 d . . . . .
C7 C 1.2078(8) 1.0211(7) 0.5422(3) 0.0509(14) Uani 1 1 d . . . . .
H7 H 1.2646 1.0447 0.5139 0.061 Uiso 1 1 calc R U . . .
C8 C 1.2211(10) 1.0852(8) 0.5849(3) 0.0585(17) Uani 1 1 d . . . . .
H8 H 1.2887 1.1588 0.5905 0.070 Uiso 1 1 calc R U . . .
C9 C 1.1163(11) 1.0210(9) 0.6182(2) 0.0582(16) Uani 1 1 d . . . . .
H9 H 1.1003 1.0446 0.6499 0.070 Uiso 1 1 calc R U . . .
C10 C 1.0398(10) 0.9160(7) 0.5962(2) 0.0538(15) Uani 1 1 d . . . . .
H10 H 0.9645 0.8560 0.6107 0.065 Uiso 1 1 calc R U . . .
C11 C 0.8896(13) 1.2575(8) 0.5499(4) 0.069(2) Uani 1 1 d . . . . .
H11 H 0.9648 1.3289 0.5503 0.083 Uiso 1 1 calc R U . . .
C12 C 0.8546(15) 1.1799(10) 0.5110(3) 0.075(2) Uani 1 1 d . . . . .
H12 H 0.9032 1.1901 0.4807 0.090 Uiso 1 1 calc R U . . .
C13 C 0.7354(12) 1.0846(10) 0.5248(3) 0.068(2) Uani 1 1 d . . . . .
H13 H 0.6895 1.0198 0.5055 0.081 Uiso 1 1 calc R U . . .
C14 C 0.6969(9) 1.1033(8) 0.5726(3) 0.0599(18) Uani 1 1 d . . . . .
H14 H 0.6201 1.0531 0.5911 0.072 Uiso 1 1 calc R U . . .
C15 C 0.7922(11) 1.2094(8) 0.5883(3) 0.0602(17) Uani 1 1 d . . . . .
H15 H 0.7912 1.2427 0.6191 0.072 Uiso 1 1 calc R U . . .
C101 C 0.5317(10) 0.8556(7) 0.3017(3) 0.0533(15) Uani 1 1 d . . . . .
C102 C 0.5794(10) 1.1128(7) 0.2966(2) 0.0536(15) Uani 1 1 d . . . . .
C103 C 0.7264(10) 0.9785(8) 0.2327(3) 0.0563(16) Uani 1 1 d . . . . .
C201 C 1.1975(9) 1.0079(7) 0.3590(2) 0.0493(14) Uani 1 1 d . . . . .
C202 C 1.1405(9) 1.0442(7) 0.2655(2) 0.0504(14) Uani 1 1 d . . . . .
C203 C 0.9837(10) 1.2025(7) 0.3214(2) 0.0542(16) Uani 1 1 d . . . . .
Fe1 Fe 0.70790(13) 0.96932(10) 0.29560(3) 0.0464(3) Uani 1 1 d . . . . .
Fe2 Fe 1.01537(14) 1.03537(10) 0.31884(3) 0.0453(3) Uani 1 1 d . . . . .
Fe3 Fe 0.96338(15) 1.07699(10) 0.56356(4) 0.0485(3) Uani 1 1 d . . . . .
N1 N 0.9686(8) 0.8074(5) 0.39268(19) 0.0493(12) Uani 1 1 d . . . . .
O101 O 0.4251(8) 0.7823(6) 0.3059(2) 0.0653(13) Uani 1 1 d . . . . .
O102 O 0.5013(9) 1.2029(6) 0.2984(2) 0.0669(14) Uani 1 1 d . . . . .
O103 O 0.7382(9) 0.9882(7) 0.1932(2) 0.0699(15) Uani 1 1 d . . . . .
O201 O 1.3139(7) 0.9912(6) 0.38297(19) 0.0587(12) Uani 1 1 d . . . . .
O202 O 1.2213(8) 1.0486(6) 0.23205(19) 0.0626(13) Uani 1 1 d . . . . .
O203 O 0.9612(9) 1.3081(5) 0.3229(2) 0.0650(13) Uani 1 1 d . . . . .
S1 S 0.7854(2) 1.02035(15) 0.36901(5) 0.0461(4) Uani 1 1 d . . . . .
S2 S 0.9429(2) 0.83874(15) 0.29783(5) 0.0473(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
C1 N1 1.441(10) . ?
C1 S1 1.829(8) . ?
C2 N1 1.433(9) . ?
C2 S2 1.845(7) . ?
C3 N1 1.485(9) . ?
C3 C4 1.492(10) . ?
C4 C5 1.319(10) . ?
C5 C6 1.465(10) . ?
C6 C7 1.426(11) . ?
C6 C10 1.438(10) . ?
C6 Fe3 2.040(7) . ?
C7 C8 1.407(11) . ?
C7 Fe3 2.033(6) . ?
C8 C9 1.415(13) . ?
C8 Fe3 2.042(7) . ?
C9 C10 1.408(12) . ?
C9 Fe3 2.035(7) . ?
C10 Fe3 2.038(7) . ?
C11 C12 1.413(15) . ?
C11 C15 1.418(13) . ?
C11 Fe3 2.040(8) . ?
C12 C13 1.414(17) . ?
C12 Fe3 2.035(8) . ?
C13 C14 1.414(13) . ?
C13 Fe3 2.050(8) . ?
C14 C15 1.414(12) . ?
C14 Fe3 2.048(7) . ?
C15 Fe3 2.041(8) . ?
C101 O101 1.128(10) . ?
C101 Fe1 1.808(8) . ?
C102 O102 1.128(10) . ?
C102 Fe1 1.812(8) . ?
C103 O103 1.138(10) . ?
C103 Fe1 1.811(8) . ?
C201 O201 1.130(9) . ?
C201 Fe2 1.816(8) . ?
C202 O202 1.136(9) . ?
C202 Fe2 1.800(7) . ?
C203 O203 1.139(10) . ?
C203 Fe2 1.798(8) . ?
Fe1 S1 2.2497(18) . ?
Fe1 S2 2.2556(19) . ?
Fe1 Fe2 2.5154(14) . ?
Fe2 S2 2.2483(18) . ?
Fe2 S1 2.2598(18) . ?

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 C1 S1 113.5(5) . . ?
N1 C2 S2 113.1(5) . . ?
N1 C3 C4 109.2(6) . . ?
C5 C4 C3 125.5(7) . . ?
C4 C5 C6 125.8(7) . . ?
C7 C6 C10 106.5(6) . . ?
C7 C6 C5 127.1(7) . . ?
C10 C6 C5 126.4(7) . . ?
C7 C6 Fe3 69.2(4) . . ?
C10 C6 Fe3 69.3(4) . . ?
C5 C6 Fe3 125.0(5) . . ?
C8 C7 C6 108.8(7) . . ?
C8 C7 Fe3 70.1(4) . . ?
C6 C7 Fe3 69.8(4) . . ?
C7 C8 C9 108.2(7) . . ?
C7 C8 Fe3 69.5(4) . . ?
C9 C8 Fe3 69.4(4) . . ?
C10 C9 C8 108.2(7) . . ?
C10 C9 Fe3 69.9(4) . . ?
C8 C9 Fe3 69.9(4) . . ?
C9 C10 C6 108.4(7) . . ?
C9 C10 Fe3 69.7(4) . . ?
C6 C10 Fe3 69.4(4) . . ?
C12 C11 C15 107.7(9) . . ?
C12 C11 Fe3 69.5(5) . . ?
C15 C11 Fe3 69.7(5) . . ?
C11 C12 C13 108.6(8) . . ?
C11 C12 Fe3 69.9(5) . . ?
C13 C12 Fe3 70.3(5) . . ?
C12 C13 C14 107.5(9) . . ?
C12 C13 Fe3 69.2(5) . . ?
C14 C13 Fe3 69.7(5) . . ?
C13 C14 C15 108.4(8) . . ?
C13 C14 Fe3 69.9(5) . . ?
C15 C14 Fe3 69.5(4) . . ?
C14 C15 C11 107.8(8) . . ?
C14 C15 Fe3 70.0(4) . . ?
C11 C15 Fe3 69.6(5) . . ?
O101 C101 Fe1 178.1(7) . . ?
O102 C102 Fe1 178.0(7) . . ?
O103 C103 Fe1 177.8(8) . . ?
O201 C201 Fe2 178.1(6) . . ?
O202 C202 Fe2 179.0(7) . . ?
O203 C203 Fe2 179.0(8) . . ?
C101 Fe1 C103 100.9(3) . . ?
C101 Fe1 C102 99.8(3) . . ?
C103 Fe1 C102 90.6(3) . . ?
C101 Fe1 S1 105.2(2) . . ?
C103 Fe1 S1 153.9(3) . . ?
C102 Fe1 S1 85.4(2) . . ?
C101 Fe1 S2 99.3(2) . . ?
C103 Fe1 S2 90.0(2) . . ?
C102 Fe1 S2 160.3(2) . . ?
S1 Fe1 S2 85.31(7) . . ?
C101 Fe1 Fe2 147.2(2) . . ?
C103 Fe1 Fe2 100.2(2) . . ?
C102 Fe1 Fe2 104.7(2) . . ?
S1 Fe1 Fe2 56.29(5) . . ?
S2 Fe1 Fe2 55.91(5) . . ?
C203 Fe2 C202 93.0(3) . . ?
C203 Fe2 C201 103.6(3) . . ?
C202 Fe2 C201 98.6(3) . . ?
C203 Fe2 S2 154.4(3) . . ?
C202 Fe2 S2 87.1(2) . . ?
C201 Fe2 S2 101.8(2) . . ?
C203 Fe2 S1 86.7(2) . . ?
C202 Fe2 S1 161.3(2) . . ?
C201 Fe2 S1 99.6(2) . . ?
S2 Fe2 S1 85.25(7) . . ?
C203 Fe2 Fe1 99.5(3) . . ?
C202 Fe2 Fe1 105.9(2) . . ?
C201 Fe2 Fe1 145.2(2) . . ?
S2 Fe2 Fe1 56.19(5) . . ?
S1 Fe2 Fe1 55.90(5) . . ?
C7 Fe3 C12 107.5(4) . . ?
C7 Fe3 C9 68.4(3) . . ?
C12 Fe3 C9 162.9(5) . . ?
C7 Fe3 C10 68.6(3) . . ?
C12 Fe3 C10 155.2(4) . . ?
C9 Fe3 C10 40.5(3) . . ?
C7 Fe3 C6 41.0(3) . . ?
C12 Fe3 C6 119.5(4) . . ?
C9 Fe3 C6 69.0(3) . . ?
C10 Fe3 C6 41.3(3) . . ?
C7 Fe3 C11 117.8(3) . . ?
C12 Fe3 C11 40.6(4) . . ?
C9 Fe3 C11 125.4(4) . . ?
C10 Fe3 C11 163.5(4) . . ?
C6 Fe3 C11 152.8(3) . . ?
C7 Fe3 C15 151.9(3) . . ?
C12 Fe3 C15 68.2(4) . . ?
C9 Fe3 C15 107.1(3) . . ?
C10 Fe3 C15 127.0(3) . . ?
C6 Fe3 C15 165.6(3) . . ?
C11 Fe3 C15 40.7(4) . . ?
C7 Fe3 C8 40.4(3) . . ?
C12 Fe3 C8 125.7(4) . . ?
C9 Fe3 C8 40.6(4) . . ?
C10 Fe3 C8 68.2(3) . . ?
C6 Fe3 C8 68.7(3) . . ?
C11 Fe3 C8 106.1(4) . . ?
C15 Fe3 C8 118.0(4) . . ?
C7 Fe3 C14 165.9(3) . . ?
C12 Fe3 C14 67.9(4) . . ?
C9 Fe3 C14 120.0(3) . . ?
C10 Fe3 C14 109.6(3) . . ?
C6 Fe3 C14 128.4(3) . . ?
C11 Fe3 C14 68.1(4) . . ?
C15 Fe3 C14 40.5(4) . . ?
C8 Fe3 C14 153.2(3) . . ?
C7 Fe3 C13 127.6(3) . . ?
C12 Fe3 C13 40.5(5) . . ?
C9 Fe3 C13 154.8(4) . . ?
C10 Fe3 C13 121.3(4) . . ?
C6 Fe3 C13 109.0(3) . . ?
C11 Fe3 C13 68.3(4) . . ?
C15 Fe3 C13 68.2(4) . . ?
C8 Fe3 C13 164.0(4) . . ?
C14 Fe3 C13 40.4(4) . . ?
C2 N1 C1 112.4(6) . . ?
C2 N1 C3 114.4(5) . . ?
C1 N1 C3 113.2(5) . . ?
C1 S1 Fe1 111.0(2) . . ?
C1 S1 Fe2 108.9(2) . . ?
Fe1 S1 Fe2 67.81(6) . . ?
C2 S2 Fe2 108.8(2) . . ?
C2 S2 Fe1 112.8(3) . . ?
Fe2 S2 Fe1 67.91(6) . . ?

_refine_diff_density_max         1.539
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.267

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_13b
_database_code_depnum_ccdc_archive 'CCDC 2308700'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2023-11-17 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H19 Fe2 N O7 Ru S2'
_chemical_formula_weight         746.32

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'
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'
Ru Ru 0.0552 3.2960 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   27.1359(15)
_cell_length_b                   8.2566(4)
_cell_length_c                   12.5739(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.619(5)
_cell_angle_gamma                90
_cell_volume                     2759.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4891
_cell_measurement_theta_min      3.2890
_cell_measurement_theta_max      69.2790

_exptl_crystal_description       block
_exptl_crystal_colour            red-orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.053
_exptl_absorpt_coefficient_mu    14.522
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.108
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13971
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.325
_diffrn_reflns_theta_max         70.611
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5114
_reflns_number_gt                3808
_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 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2022)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_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)+(0.1375P)²+7.3820P] 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         5114
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0770
_refine_ls_wR_factor_ref         0.2446
_refine_ls_wR_factor_gt          0.2135
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
C1 C 0.7075(4) 0.2525(11) 0.1109(7) 0.051(2) Uani 1 1 d . . . . .
H1A H 0.7201 0.2439 0.1902 0.061 Uiso 1 1 calc R U . . .
H1B H 0.7136 0.1472 0.0781 0.061 Uiso 1 1 calc R U . . .
C2 C 0.7266(3) 0.3886(13) -0.0485(6) 0.052(2) Uani 1 1 d . . . . .
H2A H 0.7318 0.2810 -0.0792 0.062 Uiso 1 1 calc R U . . .
H2B H 0.7520 0.4632 -0.0679 0.062 Uiso 1 1 calc R U . . .
C3 C 0.7605(4) 0.4940(12) 0.1312(7) 0.055(2) Uani 1 1 d . . . . .
C4 C 0.7733(4) 0.4765(11) 0.2525(7) 0.050(2) Uani 1 1 d . . . . .
C5 C 0.7540(4) 0.5869(14) 0.3159(8) 0.064(2) Uani 1 1 d . . . . .
H5 H 0.7303 0.6656 0.2826 0.077 Uiso 1 1 calc R U . . .
C6 C 0.7689(5) 0.5830(14) 0.4265(8) 0.072(3) Uani 1 1 d . . . . .
H6 H 0.7533 0.6534 0.4694 0.087 Uiso 1 1 calc R U . . .
C7 C 0.8061(4) 0.4793(13) 0.4771(7) 0.063(3) Uani 1 1 d . . . . .
C8 C 0.8240(4) 0.3644(14) 0.4138(8) 0.065(3) Uani 1 1 d . . . . .
H8 H 0.8478 0.2858 0.4470 0.079 Uiso 1 1 calc R U . . .
C9 C 0.8072(4) 0.3642(13) 0.3010(7) 0.058(2) Uani 1 1 d . . . . .
H9 H 0.8194 0.2851 0.2581 0.069 Uiso 1 1 calc R U . . .
C10 C 0.8205(5) 0.4971(18) 0.5960(9) 0.080(3) Uani 1 1 d . . . . .
H10 H 0.7966 0.5509 0.6294 0.097 Uiso 1 1 calc R U . . .
C11 C 0.8596(6) 0.4515(14) 0.6592(10) 0.080(3) Uani 1 1 d . . . . .
H11 H 0.8834 0.3914 0.6290 0.096 Uiso 1 1 calc R U . . .
C12 C 0.8719(4) 0.4834(13) 0.7765(7) 0.064(3) Uani 1 1 d . . . . .
C13 C 0.8478(4) 0.5864(16) 0.8408(10) 0.070(3) Uani 1 1 d . . . . .
H13 H 0.8183 0.6480 0.8151 0.084 Uiso 1 1 calc R U . . .
C14 C 0.8757(4) 0.5821(15) 0.9523(9) 0.069(3) Uani 1 1 d . . . . .
H14 H 0.8675 0.6374 1.0125 0.083 Uiso 1 1 calc R U . . .
C15 C 0.9176(4) 0.4799(13) 0.9536(8) 0.063(3) Uani 1 1 d . . . . .
H15 H 0.9427 0.4548 1.0157 0.076 Uiso 1 1 calc R U . . .
C16 C 0.9159(4) 0.4211(13) 0.8471(8) 0.064(3) Uani 1 1 d . . . . .
H16 H 0.9401 0.3515 0.8259 0.077 Uiso 1 1 calc R U . . .
C17 C 0.9415(5) 0.9347(14) 0.8682(11) 0.082(3) Uani 1 1 d . . . . .
H17 H 0.9276 1.0019 0.9160 0.098 Uiso 1 1 calc R U . . .
C18 C 0.9214(4) 0.9100(14) 0.7591(10) 0.072(3) Uani 1 1 d . . . . .
H18 H 0.8914 0.9578 0.7195 0.087 Uiso 1 1 calc R U . . .
C19 C 0.9537(5) 0.7996(15) 0.7153(11) 0.077(3) Uani 1 1 d . . . . .
H19 H 0.9492 0.7629 0.6424 0.092 Uiso 1 1 calc R U . . .
C20 C 0.9938(4) 0.7563(15) 0.8040(10) 0.069(3) Uani 1 1 d . . . . .
H20 H 1.0202 0.6827 0.8000 0.083 Uiso 1 1 calc R U . . .
C21 C 0.9876(5) 0.8401(15) 0.8974(11) 0.078(3) Uani 1 1 d . . . . .
H21 H 1.0094 0.8360 0.9667 0.093 Uiso 1 1 calc R U . . .
C101 C 0.6281(4) 0.0900(12) -0.1340(7) 0.055(2) Uani 1 1 d . . . . .
C102 C 0.5470(4) 0.2032(11) -0.0596(6) 0.049(2) Uani 1 1 d . . . . .
C103 C 0.5699(4) 0.3444(12) -0.2231(7) 0.054(2) Uani 1 1 d . . . . .
C201 C 0.5680(4) 0.5300(12) 0.0888(8) 0.058(2) Uani 1 1 d . . . . .
C202 C 0.5791(4) 0.6593(13) -0.0912(8) 0.062(2) Uani 1 1 d . . . . .
C203 C 0.6539(4) 0.6999(13) 0.0826(9) 0.063(3) Uani 1 1 d . . . . .
Fe1 Fe 0.60431(5) 0.27845(17) -0.09296(9) 0.0455(4) Uani 1 1 d . . . . .
Fe2 Fe 0.61744(5) 0.53718(15) 0.01134(9) 0.0452(4) Uani 1 1 d . . . . .
N1 N 0.7355(3) 0.3747(8) 0.0689(5) 0.0453(15) Uani 1 1 d . . . . .
O7 O 0.7755(4) 0.6155(10) 0.0894(6) 0.082(2) Uani 1 1 d . . . . .
O101 O 0.6426(3) -0.0309(9) -0.1571(6) 0.073(2) Uani 1 1 d . . . . .
O102 O 0.5097(3) 0.1616(9) -0.0409(5) 0.0657(18) Uani 1 1 d . . . . .
O103 O 0.5473(3) 0.3938(10) -0.3029(5) 0.0685(19) Uani 1 1 d . . . . .
O201 O 0.5373(3) 0.5205(10) 0.1381(6) 0.0680(18) Uani 1 1 d . . . . .
O202 O 0.5554(3) 0.7343(10) -0.1591(6) 0.075(2) Uani 1 1 d . . . . .
O203 O 0.6740(4) 0.8138(10) 0.1214(7) 0.083(2) Uani 1 1 d . . . . .
Ru1 Ru 0.92315(3) 0.67984(9) 0.84433(5) 0.0547(3) Uani 1 1 d . . . . .
S1 S 0.63884(8) 0.2897(2) 0.08520(14) 0.0441(5) Uani 1 1 d . . . . .
S2 S 0.66338(8) 0.4623(3) -0.11253(15) 0.0491(5) 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
C1 N1 1.427(12) . ?
C1 S1 1.850(10) . ?
C2 N1 1.452(10) . ?
C2 S2 1.846(9) . ?
C3 O7 1.240(12) . ?
C3 N1 1.352(12) . ?
C3 C4 1.500(12) . ?
C4 C9 1.360(14) . ?
C4 C5 1.381(15) . ?
C5 C6 1.369(14) . ?
C6 C7 1.377(17) . ?
C7 C8 1.387(17) . ?
C7 C10 1.476(14) . ?
C8 C9 1.399(13) . ?
C10 C11 1.249(19) . ?
C11 C12 1.469(15) . ?
C12 C13 1.419(17) . ?
C12 C16 1.433(15) . ?
C12 Ru1 2.195(9) . ?
C13 C14 1.453(16) . ?
C13 Ru1 2.177(11) . ?
C14 C15 1.412(17) . ?
C14 Ru1 2.202(11) . ?
C15 C16 1.417(15) . ?
C15 Ru1 2.172(10) . ?
C16 Ru1 2.146(11) . ?
C17 C18 1.386(18) . ?
C17 C21 1.458(19) . ?
C17 Ru1 2.170(11) . ?
C18 C19 1.447(19) . ?
C18 Ru1 2.178(12) . ?
C19 C20 1.438(16) . ?
C19 Ru1 2.199(12) . ?
C20 C21 1.401(19) . ?
C20 Ru1 2.173(11) . ?
C21 Ru1 2.188(11) . ?
C101 O101 1.133(12) . ?
C101 Fe1 1.799(10) . ?
C102 O102 1.137(12) . ?
C102 Fe1 1.802(10) . ?
C103 O103 1.141(11) . ?
C103 Fe1 1.797(9) . ?
C201 O201 1.137(13) . ?
C201 Fe2 1.810(12) . ?
C202 O202 1.142(12) . ?
C202 Fe2 1.795(11) . ?
C203 O203 1.145(13) . ?
C203 Fe2 1.797(11) . ?
Fe1 S1 2.249(2) . ?
Fe1 S2 2.257(3) . ?
Fe1 Fe2 2.4944(18) . ?
Fe2 S2 2.268(2) . ?
Fe2 S1 2.271(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 C1 S1 114.2(6) . . ?
N1 C2 S2 114.7(6) . . ?
O7 C3 N1 120.8(8) . . ?
O7 C3 C4 118.7(8) . . ?
N1 C3 C4 120.4(8) . . ?
C9 C4 C5 119.4(8) . . ?
C9 C4 C3 121.3(9) . . ?
C5 C4 C3 119.0(9) . . ?
C6 C5 C4 120.1(10) . . ?
C5 C6 C7 121.5(10) . . ?
C6 C7 C8 118.0(9) . . ?
C6 C7 C10 115.2(11) . . ?
C8 C7 C10 126.7(12) . . ?
C7 C8 C9 120.1(10) . . ?
C4 C9 C8 120.5(10) . . ?
C11 C10 C7 129.2(14) . . ?
C10 C11 C12 125.1(14) . . ?
C13 C12 C16 106.5(8) . . ?
C13 C12 C11 130.0(11) . . ?
C16 C12 C11 123.3(11) . . ?
C13 C12 Ru1 70.4(6) . . ?
C16 C12 Ru1 68.9(6) . . ?
C11 C12 Ru1 121.3(7) . . ?
C12 C13 C14 108.9(10) . . ?
C12 C13 Ru1 71.7(6) . . ?
C14 C13 Ru1 71.6(6) . . ?
C15 C14 C13 106.7(9) . . ?
C15 C14 Ru1 70.0(6) . . ?
C13 C14 Ru1 69.7(6) . . ?
C14 C15 C16 108.7(9) . . ?
C14 C15 Ru1 72.3(6) . . ?
C16 C15 Ru1 69.9(6) . . ?
C15 C16 C12 109.1(9) . . ?
C15 C16 Ru1 71.9(6) . . ?
C12 C16 Ru1 72.6(6) . . ?
C18 C17 C21 108.4(11) . . ?
C18 C17 Ru1 71.7(7) . . ?
C21 C17 Ru1 71.1(6) . . ?
C17 C18 C19 108.8(10) . . ?
C17 C18 Ru1 71.1(7) . . ?
C19 C18 Ru1 71.5(6) . . ?
C20 C19 C18 106.4(11) . . ?
C20 C19 Ru1 69.8(6) . . ?
C18 C19 Ru1 69.9(7) . . ?
C21 C20 C19 109.2(11) . . ?
C21 C20 Ru1 71.8(7) . . ?
C19 C20 Ru1 71.8(6) . . ?
C20 C21 C17 107.1(10) . . ?
C20 C21 Ru1 70.7(6) . . ?
C17 C21 Ru1 69.8(6) . . ?
O101 C101 Fe1 177.8(9) . . ?
O102 C102 Fe1 176.9(8) . . ?
O103 C103 Fe1 176.2(9) . . ?
O201 C201 Fe2 177.9(9) . . ?
O202 C202 Fe2 177.7(10) . . ?
O203 C203 Fe2 173.2(9) . . ?
C103 Fe1 C101 98.7(4) . . ?
C103 Fe1 C102 90.1(4) . . ?
C101 Fe1 C102 98.4(4) . . ?
C103 Fe1 S1 158.4(3) . . ?
C101 Fe1 S1 102.7(3) . . ?
C102 Fe1 S1 89.3(3) . . ?
C103 Fe1 S2 87.0(3) . . ?
C101 Fe1 S2 104.3(3) . . ?
C102 Fe1 S2 157.4(3) . . ?
S1 Fe1 S2 85.31(8) . . ?
C103 Fe1 Fe2 102.2(3) . . ?
C101 Fe1 Fe2 150.4(3) . . ?
C102 Fe1 Fe2 102.2(3) . . ?
S1 Fe1 Fe2 56.92(6) . . ?
S2 Fe1 Fe2 56.76(7) . . ?
C202 Fe2 C203 96.9(5) . . ?
C202 Fe2 C201 91.2(5) . . ?
C203 Fe2 C201 98.6(5) . . ?
C202 Fe2 S2 88.8(4) . . ?
C203 Fe2 S2 102.8(4) . . ?
C201 Fe2 S2 158.4(3) . . ?
C202 Fe2 S1 149.6(3) . . ?
C203 Fe2 S1 113.5(3) . . ?
C201 Fe2 S1 84.6(3) . . ?
S2 Fe2 S1 84.55(9) . . ?
C202 Fe2 Fe1 95.9(3) . . ?
C203 Fe2 Fe1 155.2(4) . . ?
C201 Fe2 Fe1 102.2(3) . . ?
S2 Fe2 Fe1 56.34(7) . . ?
S1 Fe2 Fe1 56.09(6) . . ?
C3 N1 C1 122.9(7) . . ?
C3 N1 C2 119.5(7) . . ?
C1 N1 C2 116.1(7) . . ?
C16 Ru1 C17 169.3(5) . . ?
C16 Ru1 C15 38.3(4) . . ?
C17 Ru1 C15 133.8(5) . . ?
C16 Ru1 C20 112.4(5) . . ?
C17 Ru1 C20 64.0(5) . . ?
C15 Ru1 C20 123.0(4) . . ?
C16 Ru1 C13 63.8(5) . . ?
C17 Ru1 C13 122.4(5) . . ?
C15 Ru1 C13 63.8(4) . . ?
C20 Ru1 C13 165.2(5) . . ?
C16 Ru1 C18 152.1(4) . . ?
C17 Ru1 C18 37.2(5) . . ?
C15 Ru1 C18 167.7(5) . . ?
C20 Ru1 C18 64.1(4) . . ?
C13 Ru1 C18 111.9(4) . . ?
C16 Ru1 C21 131.9(5) . . ?
C17 Ru1 C21 39.1(5) . . ?
C15 Ru1 C21 114.8(4) . . ?
C20 Ru1 C21 37.5(5) . . ?
C13 Ru1 C21 155.6(5) . . ?
C18 Ru1 C21 63.8(5) . . ?
C16 Ru1 C12 38.5(4) . . ?
C17 Ru1 C12 151.7(5) . . ?
C15 Ru1 C12 64.2(4) . . ?
C20 Ru1 C12 130.1(5) . . ?
C13 Ru1 C12 37.9(5) . . ?
C18 Ru1 C12 120.3(4) . . ?
C21 Ru1 C12 166.2(5) . . ?
C16 Ru1 C19 120.6(5) . . ?
C17 Ru1 C19 63.6(5) . . ?
C15 Ru1 C19 153.2(5) . . ?
C20 Ru1 C19 38.4(4) . . ?
C13 Ru1 C19 129.5(4) . . ?
C18 Ru1 C19 38.6(5) . . ?
C21 Ru1 C19 63.7(5) . . ?
C12 Ru1 C19 110.4(4) . . ?
C16 Ru1 C14 63.8(4) . . ?
C17 Ru1 C14 114.6(5) . . ?
C15 Ru1 C14 37.6(4) . . ?
C20 Ru1 C14 154.5(4) . . ?
C13 Ru1 C14 38.8(4) . . ?
C18 Ru1 C14 131.7(5) . . ?
C21 Ru1 C14 124.3(5) . . ?
C12 Ru1 C14 64.2(4) . . ?
C19 Ru1 C14 166.6(5) . . ?
C1 S1 Fe1 111.7(3) . . ?
C1 S1 Fe2 112.7(3) . . ?
Fe1 S1 Fe2 66.98(7) . . ?
C2 S2 Fe1 110.4(3) . . ?
C2 S2 Fe2 112.4(3) . . ?
Fe1 S2 Fe2 66.90(8) . . ?

_refine_diff_density_max         1.142
_refine_diff_density_min         -1.666
_refine_diff_density_rms         0.173

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_12c
_database_code_depnum_ccdc_archive 'CCDC 2308699'
loop_
_audit_author_name
_audit_author_address
'Javier A. Cabeza'
;Universidad de Oviedo
Spain
;
_audit_update_record             
;
2023-11-17 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H14 Fe2 Mn N O9 S2'
_chemical_formula_weight         691.12

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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.1461(4)
_cell_length_b                   10.6933(6)
_cell_length_c                   13.8344(7)
_cell_angle_alpha                87.141(4)
_cell_angle_beta                 89.136(4)
_cell_angle_gamma                78.009(4)
_cell_volume                     1321.85(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7243
_cell_measurement_theta_min      4.2260
_cell_measurement_theta_max      69.5270

_exptl_crystal_description       block
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             692
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.138
_exptl_crystal_size_rad          0.15
_exptl_absorpt_coefficient_mu    14.467
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_correction_T_min  0.00421
_exptl_absorpt_correction_T_max  0.05473
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11155
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.198
_diffrn_reflns_theta_max         69.685
_diffrn_reflns_theta_full        67.680
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             4865
_reflns_number_gt                4463
_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 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_cell_refinement       
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_data_reduction        
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    
'MERCURY (Cambridge Crystallographic Data Centre: Cambridge, UK, 2022)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'

_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)+(0.1415P)²] 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         4865
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.1859
_refine_ls_wR_factor_gt          0.1749
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_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
C1 C 0.7112(5) -0.1271(5) 0.8524(3) 0.0706(10) Uani 1 1 d . . . . .
H1A H 0.7431 -0.2215 0.8582 0.085 Uiso 1 1 calc R U . . .
H1B H 0.6640 -0.0985 0.9146 0.085 Uiso 1 1 calc R U . . .
C2 C 0.5240(5) 0.0353(5) 0.7795(4) 0.0753(11) Uani 1 1 d . . . . .
H2A H 0.4796 0.0496 0.8447 0.090 Uiso 1 1 calc R U . . .
H2B H 0.4406 0.0479 0.7328 0.090 Uiso 1 1 calc R U . . .
C3 C 0.6159(5) -0.1623(4) 0.6933(3) 0.0664(9) Uani 1 1 d . . . . .
C4 C 0.5139(5) -0.1287(5) 0.6179(4) 0.0768(11) Uani 1 1 d . . . . .
H4 H 0.4399 -0.0522 0.6210 0.092 Uiso 1 1 calc R U . . .
C5 C 0.5171(6) -0.2034(5) 0.5388(4) 0.0811(12) Uani 1 1 d . . . . .
H5 H 0.4441 -0.1776 0.4896 0.097 Uiso 1 1 calc R U . . .
C6 C 0.6231(6) -0.3140(5) 0.5293(3) 0.0759(11) Uani 1 1 d . . . . .
C7 C 0.7292(6) -0.3471(5) 0.6025(4) 0.0780(11) Uani 1 1 d . . . . .
H7 H 0.8052 -0.4220 0.5972 0.094 Uiso 1 1 calc R U . . .
C8 C 0.7273(6) -0.2742(5) 0.6828(4) 0.0743(10) Uani 1 1 d . . . . .
H8 H 0.8015 -0.2996 0.7312 0.089 Uiso 1 1 calc R U . . .
C9 C 0.6151(6) -0.3919(5) 0.4455(4) 0.0788(11) Uani 1 1 d . . . . .
H9 H 0.5258 -0.3698 0.4087 0.095 Uiso 1 1 calc R U . . .
C10 C 0.7161(6) -0.4880(5) 0.4154(4) 0.0755(10) Uani 1 1 d . . . . .
H10 H 0.8078 -0.5111 0.4496 0.091 Uiso 1 1 calc R U . . .
C11 C 0.6953(6) -0.5620(4) 0.3320(3) 0.0727(10) Uani 1 1 d . . . . .
C12 C 0.8012(6) -0.6686(5) 0.3017(4) 0.0755(11) Uani 1 1 d . . . . .
H12 H 0.8963 -0.7009 0.3301 0.091 Uiso 1 1 calc R U . . .
C13 C 0.7423(6) -0.7190(4) 0.2222(4) 0.0747(10) Uani 1 1 d . . . . .
H13 H 0.7907 -0.7917 0.1886 0.090 Uiso 1 1 calc R U . . .
C14 C 0.6006(6) -0.6441(5) 0.2010(4) 0.0757(11) Uani 1 1 d . . . . .
H14 H 0.5358 -0.6568 0.1510 0.091 Uiso 1 1 calc R U . . .
C15 C 0.5720(5) -0.5455(5) 0.2686(4) 0.0746(10) Uani 1 1 d . . . . .
H15 H 0.4848 -0.4796 0.2708 0.089 Uiso 1 1 calc R U . . .
C101 C 0.7857(5) 0.3248(5) 0.8508(4) 0.0755(10) Uani 1 1 d . . . . .
C102 C 1.0006(5) 0.1437(4) 0.9073(3) 0.0681(9) Uani 1 1 d . . . . .
C103 C 0.7111(6) 0.1398(5) 0.9746(3) 0.0731(10) Uani 1 1 d . . . . .
C201 C 1.0646(5) 0.0432(4) 0.6995(3) 0.0662(9) Uani 1 1 d . . . . .
C202 C 0.8645(6) 0.2211(5) 0.6301(4) 0.0803(11) Uani 1 1 d . . . . .
C203 C 0.8482(5) -0.0198(5) 0.5928(3) 0.0697(10) Uani 1 1 d . . . . .
C301 C 0.8382(8) -0.3983(6) 0.2238(4) 0.0964(17) Uani 1 1 d . . . . .
C302 C 0.9228(6) -0.5856(5) 0.1089(4) 0.0785(11) Uani 1 1 d . . . . .
C303 C 0.6666(6) -0.4307(6) 0.0852(4) 0.0863(13) Uani 1 1 d . . . . .
Fe1 Fe 0.81355(7) 0.15342(6) 0.86344(4) 0.0611(2) Uani 1 1 d . . . . .
Fe2 Fe 0.86609(6) 0.07354(6) 0.69653(4) 0.0582(2) Uani 1 1 d . . . . .
Mn1 Mn 0.76367(7) -0.52828(6) 0.18370(5) 0.0639(2) Uani 1 1 d . . . . .
N1 N 0.6023(4) -0.0939(4) 0.7775(3) 0.0708(8) Uani 1 1 d . . . . .
O101 O 0.7676(5) 0.4344(4) 0.8433(4) 0.1016(12) Uani 1 1 d . . . . .
O102 O 1.1200(4) 0.1358(4) 0.9314(3) 0.0827(9) Uani 1 1 d . . . . .
O103 O 0.6440(5) 0.1267(4) 1.0429(3) 0.0880(9) Uani 1 1 d . . . . .
O201 O 1.1914(4) 0.0251(4) 0.7035(3) 0.0890(10) Uani 1 1 d . . . . .
O202 O 0.8653(7) 0.3156(5) 0.5885(4) 0.1213(16) Uani 1 1 d . . . . .
O203 O 0.8468(5) -0.0716(4) 0.5239(3) 0.0931(11) Uani 1 1 d . . . . .
O301 O 0.8827(9) -0.3161(6) 0.2523(4) 0.148(3) Uani 1 1 d . . . . .
O302 O 1.0234(5) -0.6254(4) 0.0614(4) 0.1067(14) Uani 1 1 d . . . . .
O303 O 0.6022(6) -0.3672(6) 0.0246(4) 0.1223(17) Uani 1 1 d . . . . .
S1 S 0.88062(10) -0.05657(9) 0.83254(7) 0.0608(3) Uani 1 1 d . . . . .
S2 S 0.63565(10) 0.16065(10) 0.75069(7) 0.0656(3) 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
C1 N1 1.428(6) . ?
C1 S1 1.870(4) . ?
C2 N1 1.420(6) . ?
C2 S2 1.871(5) . ?
C3 C4 1.392(7) . ?
C3 N1 1.397(6) . ?
C3 C8 1.413(7) . ?
C4 C5 1.384(7) . ?
C5 C6 1.375(8) . ?
C6 C7 1.395(8) . ?
C6 C9 1.472(7) . ?
C7 C8 1.387(7) . ?
C9 C10 1.311(8) . ?
C10 C11 1.469(7) . ?
C11 C12 1.410(7) . ?
C11 C15 1.415(7) . ?
C11 Mn1 2.170(4) . ?
C12 C13 1.410(7) . ?
C12 Mn1 2.142(5) . ?
C13 C14 1.402(8) . ?
C13 Mn1 2.130(4) . ?
C14 C15 1.426(7) . ?
C14 Mn1 2.132(4) . ?
C15 Mn1 2.130(5) . ?
C101 O101 1.148(6) . ?
C101 Fe1 1.797(5) . ?
C102 O102 1.131(6) . ?
C102 Fe1 1.805(5) . ?
C103 O103 1.137(6) . ?
C103 Fe1 1.804(5) . ?
C201 O201 1.138(6) . ?
C201 Fe2 1.777(4) . ?
C202 O202 1.139(7) . ?
C202 Fe2 1.784(5) . ?
C203 O203 1.128(6) . ?
C203 Fe2 1.817(5) . ?
C301 O301 1.133(7) . ?
C301 Mn1 1.785(6) . ?
C302 O302 1.143(7) . ?
C302 Mn1 1.792(5) . ?
C303 O303 1.142(7) . ?
C303 Mn1 1.801(6) . ?
Fe1 S2 2.2580(11) . ?
Fe1 S1 2.2620(11) . ?
Fe1 Fe2 2.5070(8) . ?
Fe2 S2 2.2533(11) . ?
Fe2 S1 2.2723(10) . ?

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 C1 S1 114.2(3) . . ?
N1 C2 S2 116.5(3) . . ?
C4 C3 N1 121.6(4) . . ?
C4 C3 C8 116.4(4) . . ?
N1 C3 C8 121.8(4) . . ?
C5 C4 C3 122.0(5) . . ?
C6 C5 C4 121.7(5) . . ?
C5 C6 C7 117.1(5) . . ?
C5 C6 C9 118.7(5) . . ?
C7 C6 C9 124.2(5) . . ?
C8 C7 C6 122.0(5) . . ?
C7 C8 C3 120.6(5) . . ?
C10 C9 C6 128.0(5) . . ?
C9 C10 C11 123.7(5) . . ?
C12 C11 C15 107.0(4) . . ?
C12 C11 C10 123.9(5) . . ?
C15 C11 C10 129.1(5) . . ?
C12 C11 Mn1 69.9(3) . . ?
C15 C11 Mn1 69.3(3) . . ?
C10 C11 Mn1 126.7(3) . . ?
C11 C12 C13 108.6(4) . . ?
C11 C12 Mn1 72.0(3) . . ?
C13 C12 Mn1 70.2(3) . . ?
C14 C13 C12 108.7(4) . . ?
C14 C13 Mn1 70.9(3) . . ?
C12 C13 Mn1 71.2(3) . . ?
C13 C14 C15 107.1(4) . . ?
C13 C14 Mn1 70.7(3) . . ?
C15 C14 Mn1 70.4(2) . . ?
C11 C15 C14 108.7(4) . . ?
C11 C15 Mn1 72.3(3) . . ?
C14 C15 Mn1 70.5(3) . . ?
O101 C101 Fe1 179.6(5) . . ?
O102 C102 Fe1 177.3(4) . . ?
O103 C103 Fe1 176.8(4) . . ?
O201 C201 Fe2 178.3(4) . . ?
O202 C202 Fe2 179.0(6) . . ?
O203 C203 Fe2 173.2(4) . . ?
O301 C301 Mn1 177.6(5) . . ?
O302 C302 Mn1 178.1(5) . . ?
O303 C303 Mn1 178.0(6) . . ?
C101 Fe1 C103 99.0(2) . . ?
C101 Fe1 C102 90.5(2) . . ?
C103 Fe1 C102 101.8(2) . . ?
C101 Fe1 S2 88.98(16) . . ?
C103 Fe1 S2 102.03(16) . . ?
C102 Fe1 S2 155.91(14) . . ?
C101 Fe1 S1 161.90(17) . . ?
C103 Fe1 S1 98.95(16) . . ?
C102 Fe1 S1 88.02(15) . . ?
S2 Fe1 S1 85.13(4) . . ?
C101 Fe1 Fe2 106.14(17) . . ?
C103 Fe1 Fe2 145.55(15) . . ?
C102 Fe1 Fe2 101.13(14) . . ?
S2 Fe1 Fe2 56.15(3) . . ?
S1 Fe1 Fe2 56.63(3) . . ?
C201 Fe2 C202 89.8(2) . . ?
C201 Fe2 C203 97.4(2) . . ?
C202 Fe2 C203 96.5(2) . . ?
C201 Fe2 S2 153.87(15) . . ?
C202 Fe2 S2 87.68(19) . . ?
C203 Fe2 S2 108.74(14) . . ?
C201 Fe2 S1 86.39(14) . . ?
C202 Fe2 S1 154.87(18) . . ?
C203 Fe2 S1 108.58(15) . . ?
S2 Fe2 S1 85.00(4) . . ?
C201 Fe2 Fe1 98.70(15) . . ?
C202 Fe2 Fe1 100.03(18) . . ?
C203 Fe2 Fe1 156.88(13) . . ?
S2 Fe2 Fe1 56.33(3) . . ?
S1 Fe2 Fe1 56.24(3) . . ?
C301 Mn1 C302 93.4(3) . . ?
C301 Mn1 C303 91.9(3) . . ?
C302 Mn1 C303 92.1(2) . . ?
C301 Mn1 C13 142.9(3) . . ?
C302 Mn1 C13 91.1(2) . . ?
C303 Mn1 C13 124.7(2) . . ?
C301 Mn1 C15 109.3(2) . . ?
C302 Mn1 C15 155.0(2) . . ?
C303 Mn1 C15 97.3(2) . . ?
C13 Mn1 C15 64.52(19) . . ?
C301 Mn1 C14 148.3(2) . . ?
C302 Mn1 C14 117.4(2) . . ?
C303 Mn1 C14 94.0(2) . . ?
C13 Mn1 C14 38.4(2) . . ?
C15 Mn1 C14 39.09(19) . . ?
C301 Mn1 C12 104.6(2) . . ?
C302 Mn1 C12 100.7(2) . . ?
C303 Mn1 C12 158.3(2) . . ?
C13 Mn1 C12 38.5(2) . . ?
C15 Mn1 C12 64.2(2) . . ?
C14 Mn1 C12 64.60(19) . . ?
C301 Mn1 C11 88.1(2) . . ?
C302 Mn1 C11 136.7(2) . . ?
C303 Mn1 C11 131.1(2) . . ?
C13 Mn1 C11 64.36(19) . . ?
C15 Mn1 C11 38.4(2) . . ?
C14 Mn1 C11 64.89(18) . . ?
C12 Mn1 C11 38.2(2) . . ?
C3 N1 C2 122.1(4) . . ?
C3 N1 C1 120.6(4) . . ?
C2 N1 C1 112.6(4) . . ?
C1 S1 Fe1 107.20(16) . . ?
C1 S1 Fe2 112.92(15) . . ?
Fe1 S1 Fe2 67.13(3) . . ?
C2 S2 Fe2 111.36(14) . . ?
C2 S2 Fe1 110.71(18) . . ?
Fe2 S2 Fe1 67.52(3) . . ?

_refine_diff_density_max         1.130
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.212

_shelxl_version_number           2014-3

