# 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_MW509
_database_code_depnum_ccdc_archive 'CCDC 2204517'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-30 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 16 mai 2022                                              #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H26 Fe O2 S2'
_chemical_formula_sum            'C18 H26 Fe O2 S2'
_chemical_formula_weight         394.36
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'
_space_group_IT_number           5
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.440(3)
_cell_length_b                   10.1792(16)
_cell_length_c                   5.9928(9)
_cell_angle_alpha                90
_cell_angle_beta                 103.022(5)
_cell_angle_gamma                90
_cell_volume                     1096.0(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    8627
_cell_measurement_theta_min      2.2996
_cell_measurement_theta_max      27.4966
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0006942
_diffrn_orient_matrix_UB_21      -0.0350522
_diffrn_orient_matrix_UB_31      -0.0432310
_diffrn_orient_matrix_UB_12      -0.0891205
_diffrn_orient_matrix_UB_22      0.0327958
_diffrn_orient_matrix_UB_32      -0.0251601
_diffrn_orient_matrix_UB_13      0.0696983
_diffrn_orient_matrix_UB_23      0.0927368
_diffrn_orient_matrix_UB_33      -0.1260002


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.190
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             416
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_T_max  0.845

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2021.10-0       #
# Number of scans            :        4                                        #
# Total number of frames [*] :      386                                        #
# Total length of scans  [*] :   386.00 (deg.)                                 #
# Rotation speed         [*] :    10.00 sec./deg.                              #
# Total exposition time  [*] :      1 h   4.3 min.                             #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     1.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Phi     10.0  1.00    34.0   192  192.0    0.1  270.3  156.0   24.0 150.0 #
#  3 Omega   10.0  1.00    34.0    97   97.0    0.1    2.7    0.0  -44.5 150.0 #
#  4 Omega   10.0  1.00    34.0    97   97.0    0.1    2.7   72.0  -44.5 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0348
_diffrn_reflns_av_r_equivalents  0.0293
_diffrn_reflns_number            7342
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         4.004
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.963
_reflns_number_total             2220
_reflns_number_gt                2213
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_max     0.779
_reflns_Friedel_fraction_full    0.818

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0731P)²+1.0477P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2220
_refine_ls_number_parameters     108
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0330
_refine_ls_wR_factor_ref         0.0991
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 
;
Flack x determined using 925 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(9)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.500000 0.75045(4) 1.000000 0.01826(19) Uani 1 2 d S T P . .
C1 C 0.39240(17) 0.7559(5) 0.8134(6) 0.0253(6) Uani 1 1 d . . . . .
H1 H 0.377313 0.757350 0.651067 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4060(2) 0.8657(5) 0.9576(8) 0.0315(9) Uani 1 1 d . . . . .
H2 H 0.401200 0.954731 0.909088 0.038 Uiso 1 1 calc R U . . .
C3 C 0.4285(2) 0.8218(5) 1.1902(8) 0.0317(9) Uani 1 1 d . . . . .
H3 H 0.440956 0.876485 1.321722 0.038 Uiso 1 1 calc R U . . .
C4 C 0.4288(2) 0.6833(4) 1.1901(6) 0.0238(7) Uani 1 1 d . . . . .
H4 H 0.441961 0.628016 1.320663 0.029 Uiso 1 1 calc R U . . .
C5 C 0.4053(2) 0.6410(4) 0.9547(6) 0.0205(7) Uani 1 1 d . . . . .
S1 S 0.40120(5) 0.47744(9) 0.85823(14) 0.0228(2) Uani 1 1 d . . . . .
O6 O 0.40747(19) 0.4828(3) 0.6124(5) 0.0371(7) Uani 1 1 d . . . . .
C7 C 0.3028(2) 0.4389(4) 0.8533(6) 0.0258(7) Uani 1 1 d . . . . .
C8 C 0.2507(2) 0.5335(6) 0.6982(7) 0.0399(10) Uani 1 1 d . . . . .
H8A H 0.264563 0.539213 0.550048 0.060 Uiso 1 1 calc R U . . .
H8B H 0.254452 0.620600 0.769492 0.060 Uiso 1 1 calc R U . . .
H8C H 0.199361 0.501559 0.675168 0.060 Uiso 1 1 calc R U . . .
C9 C 0.2936(2) 0.4432(5) 1.0988(7) 0.0359(10) Uani 1 1 d . . . . .
H9A H 0.242504 0.418774 1.102709 0.054 Uiso 1 1 calc R U . . .
H9B H 0.303979 0.532224 1.159855 0.054 Uiso 1 1 calc R U . . .
H9C H 0.328437 0.381323 1.192212 0.054 Uiso 1 1 calc R U . . .
C10 C 0.2923(3) 0.3006(5) 0.7580(9) 0.0425(11) Uani 1 1 d . . . . .
H10A H 0.331950 0.243949 0.843471 0.064 Uiso 1 1 calc R U . . .
H10B H 0.294340 0.301645 0.596047 0.064 Uiso 1 1 calc R U . . .
H10C H 0.243875 0.266772 0.772984 0.064 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C5 2.038(4) . ?
Fe1 C5 2.038(4) 2_657 ?
Fe1 C4 2.041(4) 2_657 ?
Fe1 C4 2.041(4) . ?
Fe1 C1 2.047(3) . ?
Fe1 C1 2.047(3) 2_657 ?
Fe1 C2 2.060(4) . ?
Fe1 C2 2.060(4) 2_657 ?
Fe1 C3 2.060(4) . ?
Fe1 C3 2.060(4) 2_657 ?
C1 C2 1.400(6) . ?
C1 C5 1.432(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.434(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.409(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.445(5) . ?
C4 H4 0.9500 . ?
C5 S1 1.758(4) . ?
S1 O6 1.504(3) . ?
S1 C7 1.851(4) . ?
C7 C10 1.515(6) . ?
C7 C9 1.519(5) . ?
C7 C8 1.520(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

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
C5 Fe1 C5 113.7(2) . 2_657 ?
C5 Fe1 C4 112.50(15) . 2_657 ?
C5 Fe1 C4 41.51(14) 2_657 2_657 ?
C5 Fe1 C4 41.51(15) . . ?
C5 Fe1 C4 112.50(15) 2_657 . ?
C4 Fe1 C4 140.9(2) 2_657 . ?
C5 Fe1 C1 41.04(15) . . ?
C5 Fe1 C1 141.61(17) 2_657 . ?
C4 Fe1 C1 111.76(15) 2_657 . ?
C4 Fe1 C1 69.35(14) . . ?
C5 Fe1 C1 141.61(17) . 2_657 ?
C5 Fe1 C1 41.04(15) 2_657 2_657 ?
C4 Fe1 C1 69.35(14) 2_657 2_657 ?
C4 Fe1 C1 111.76(15) . 2_657 ?
C1 Fe1 C1 176.9(3) . 2_657 ?
C5 Fe1 C2 67.85(14) . . ?
C5 Fe1 C2 178.4(2) 2_657 . ?
C4 Fe1 C2 138.68(17) 2_657 . ?
C4 Fe1 C2 68.30(18) . . ?
C1 Fe1 C2 39.86(18) . . ?
C1 Fe1 C2 137.46(18) 2_657 . ?
C5 Fe1 C2 178.39(19) . 2_657 ?
C5 Fe1 C2 67.85(14) 2_657 2_657 ?
C4 Fe1 C2 68.30(18) 2_657 2_657 ?
C4 Fe1 C2 138.68(17) . 2_657 ?
C1 Fe1 C2 137.46(18) . 2_657 ?
C1 Fe1 C2 39.86(18) 2_657 2_657 ?
C2 Fe1 C2 110.6(3) . 2_657 ?
C5 Fe1 C3 68.28(16) . . ?
C5 Fe1 C3 139.06(16) 2_657 . ?
C4 Fe1 C3 178.9(2) 2_657 . ?
C4 Fe1 C3 40.19(15) . . ?
C1 Fe1 C3 68.29(16) . . ?
C1 Fe1 C3 110.54(16) 2_657 . ?
C2 Fe1 C3 40.72(19) . . ?
C2 Fe1 C3 110.90(18) 2_657 . ?
C5 Fe1 C3 139.06(17) . 2_657 ?
C5 Fe1 C3 68.28(16) 2_657 2_657 ?
C4 Fe1 C3 40.19(15) 2_657 2_657 ?
C4 Fe1 C3 178.9(2) . 2_657 ?
C1 Fe1 C3 110.55(16) . 2_657 ?
C1 Fe1 C3 68.29(16) 2_657 2_657 ?
C2 Fe1 C3 110.90(18) . 2_657 ?
C2 Fe1 C3 40.72(19) 2_657 2_657 ?
C3 Fe1 C3 138.7(3) . 2_657 ?
C2 C1 C5 107.7(3) . . ?
C2 C1 Fe1 70.6(2) . . ?
C5 C1 Fe1 69.1(2) . . ?
C2 C1 H1 126.1 . . ?
C5 C1 H1 126.1 . . ?
Fe1 C1 H1 125.7 . . ?
C1 C2 C3 108.9(4) . . ?
C1 C2 Fe1 69.6(2) . . ?
C3 C2 Fe1 69.6(2) . . ?
C1 C2 H2 125.6 . . ?
C3 C2 H2 125.6 . . ?
Fe1 C2 H2 126.8 . . ?
C4 C3 C2 108.2(4) . . ?
C4 C3 Fe1 69.2(2) . . ?
C2 C3 Fe1 69.6(2) . . ?
C4 C3 H3 125.9 . . ?
C2 C3 H3 125.9 . . ?
Fe1 C3 H3 126.8 . . ?
C3 C4 C5 107.4(4) . . ?
C3 C4 Fe1 70.6(2) . . ?
C5 C4 Fe1 69.1(2) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 H4 126.3 . . ?
Fe1 C4 H4 125.5 . . ?
C1 C5 C4 107.9(3) . . ?
C1 C5 S1 126.2(3) . . ?
C4 C5 S1 125.8(3) . . ?
C1 C5 Fe1 69.8(2) . . ?
C4 C5 Fe1 69.4(2) . . ?
S1 C5 Fe1 122.25(19) . . ?
O6 S1 C5 106.27(18) . . ?
O6 S1 C7 106.48(18) . . ?
C5 S1 C7 100.09(18) . . ?
C10 C7 C9 111.1(3) . . ?
C10 C7 C8 110.4(4) . . ?
C9 C7 C8 112.4(4) . . ?
C10 C7 S1 104.1(3) . . ?
C9 C7 S1 107.5(2) . . ?
C8 C7 S1 111.0(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
C5 C1 C2 C3 0.7(4) . . . . ?
Fe1 C1 C2 C3 -58.7(3) . . . . ?
C5 C1 C2 Fe1 59.4(2) . . . . ?
C1 C2 C3 C4 0.0(5) . . . . ?
Fe1 C2 C3 C4 -58.6(3) . . . . ?
C1 C2 C3 Fe1 58.6(3) . . . . ?
C2 C3 C4 C5 -0.7(5) . . . . ?
Fe1 C3 C4 C5 -59.6(3) . . . . ?
C2 C3 C4 Fe1 58.9(3) . . . . ?
C2 C1 C5 C4 -1.1(4) . . . . ?
Fe1 C1 C5 C4 59.1(2) . . . . ?
C2 C1 C5 S1 -176.1(3) . . . . ?
Fe1 C1 C5 S1 -115.8(3) . . . . ?
C2 C1 C5 Fe1 -60.3(2) . . . . ?
C3 C4 C5 C1 1.2(4) . . . . ?
Fe1 C4 C5 C1 -59.4(2) . . . . ?
C3 C4 C5 S1 176.2(3) . . . . ?
Fe1 C4 C5 S1 115.6(3) . . . . ?
C3 C4 C5 Fe1 60.6(3) . . . . ?
C1 C5 S1 O6 18.5(4) . . . . ?
C4 C5 S1 O6 -155.6(3) . . . . ?
Fe1 C5 S1 O6 -68.9(3) . . . . ?
C1 C5 S1 C7 -92.1(3) . . . . ?
C4 C5 S1 C7 93.8(3) . . . . ?
Fe1 C5 S1 C7 -179.6(2) . . . . ?
O6 S1 C7 C10 66.4(3) . . . . ?
C5 S1 C7 C10 176.8(3) . . . . ?
O6 S1 C7 C9 -175.7(3) . . . . ?
C5 S1 C7 C9 -65.3(3) . . . . ?
O6 S1 C7 C8 -52.4(3) . . . . ?
C5 S1 C7 C8 58.0(3) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: sqz.res
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .FAB SHELXL file: sqz.fab
#...............................................................................


####################################################################### 
# 
# 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_MW606_2
_database_code_depnum_ccdc_archive 'CCDC 2204520'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-31 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 21 mars 2022                                             #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C20 H30 Fe O4 S2'
_chemical_formula_sum            'C20 H30 Fe O4 S2'
_chemical_formula_weight         454.41
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
_space_group_IT_number           92
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   9.7712(5)
_cell_length_b                   9.7712
_cell_length_c                   22.4446(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2142.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3409
_cell_measurement_theta_min      2.2733
_cell_measurement_theta_max      26.3161
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0739637
_diffrn_orient_matrix_UB_21      0.0706454
_diffrn_orient_matrix_UB_31      -0.0035232
_diffrn_orient_matrix_UB_12      -0.0057779
_diffrn_orient_matrix_UB_22      -0.0009537
_diffrn_orient_matrix_UB_32      0.1021740
_diffrn_orient_matrix_UB_13      0.0306906
_diffrn_orient_matrix_UB_23      0.0322337
_diffrn_orient_matrix_UB_33      0.0020364


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       diamand
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_min          0.280
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             960
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_T_max  0.773

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS 2014.5.0.0/23-May-2014 && APEX2_2014.11-0   #
# Number of scans            :        3                                        #
# Total number of frames     :      201                                        #
# Total length of scans      :   201.00 (deg.)                                 #
# Rotation speed             :  ?                                              #
# Total exposition time      :         33.5 min.                               #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Omega   10.0  1.00    35.0   108  108.0   16.0   14.9  154.4  -57.1 250.0 #
#  2 Omega   10.0  1.00    35.0    93   93.0  344.0  343.0  340.0  -27.8 250.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_detector_area_resol_mean 8.33
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0367
_diffrn_reflns_av_r_equivalents  0.0351
_diffrn_reflns_number            10117
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.764
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             2461
_reflns_number_gt                2170
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.648
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²+1.0459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018_3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0284(17)
_refine_ls_number_reflns         2461
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.0764
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
Flack x determined using 758 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.033(11)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.76709(4) 0.76709(4) 0.500000 0.0300(2) Uani 1 2 d S T P . .
C1 C 0.5927(3) 0.8771(3) 0.50673(13) 0.0316(7) Uani 1 1 d . . . . .
C2 C 0.7064(4) 0.9654(3) 0.4972(2) 0.0501(10) Uani 1 1 d . . . . .
H2 H 0.736823 1.036176 0.522945 0.060 Uiso 1 1 calc R U . . .
C3 C 0.7655(5) 0.9279(4) 0.4420(2) 0.0677(14) Uani 1 1 d . . . . .
H3 H 0.842818 0.969842 0.424048 0.081 Uiso 1 1 calc R U . . .
C4 C 0.6912(5) 0.8193(5) 0.41867(16) 0.0629(14) Uani 1 1 d . . . . .
H4 H 0.710416 0.775255 0.381883 0.075 Uiso 1 1 calc R U . . .
C5 C 0.5822(4) 0.7835(4) 0.45760(15) 0.0437(9) Uani 1 1 d . . . . .
C6 C 0.4771(5) 0.6747(5) 0.4463(3) 0.0835(18) Uani 1 1 d . . . . .
H6A H 0.465229 0.618688 0.482711 0.100 Uiso 1 1 calc R U . . .
H6B H 0.388148 0.718235 0.436973 0.100 Uiso 1 1 calc R U . . .
O7 O 0.5167(5) 0.5898(5) 0.3986(2) 0.126(2) Uani 1 1 d . . . . .
H7 H 0.581(8) 0.548(7) 0.407(3) 0.151 Uiso 1 1 d . U . . .
S1 S 0.49949(10) 0.88534(11) 0.57373(4) 0.0428(3) Uani 1 1 d . . . . .
O8 O 0.4358(3) 0.7481(3) 0.58284(15) 0.0769(11) Uani 1 1 d . . . . .
C9 C 0.3569(4) 1.0019(5) 0.55476(17) 0.0498(10) Uani 1 1 d . . . . .
C10 C 0.2759(4) 0.9459(5) 0.5021(2) 0.0756(14) Uani 1 1 d . . . . .
H10A H 0.247669 0.851597 0.510572 0.113 Uiso 1 1 calc R U . . .
H10B H 0.333276 0.947290 0.466306 0.113 Uiso 1 1 calc R U . . .
H10C H 0.194595 1.002670 0.495590 0.113 Uiso 1 1 calc R U . . .
C11 C 0.2722(6) 1.0072(6) 0.6114(2) 0.0956(19) Uani 1 1 d . . . . .
H11A H 0.197699 1.073469 0.606526 0.143 Uiso 1 1 calc R U . . .
H11B H 0.330438 1.035206 0.644828 0.143 Uiso 1 1 calc R U . . .
H11C H 0.233684 0.916511 0.619539 0.143 Uiso 1 1 calc R U . . .
C12 C 0.4195(5) 1.1406(4) 0.5411(2) 0.0609(12) Uani 1 1 d . . . . .
H12A H 0.346616 1.208949 0.537322 0.091 Uiso 1 1 calc R U . . .
H12B H 0.470764 1.135373 0.503606 0.091 Uiso 1 1 calc R U . . .
H12C H 0.481464 1.166925 0.573417 0.091 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C1 2.020(3) 7_556 ?
Fe1 C1 2.020(3) . ?
Fe1 C2 2.027(3) 7_556 ?
Fe1 C2 2.027(3) . ?
Fe1 C4 2.035(4) 7_556 ?
Fe1 C4 2.035(4) . ?
Fe1 C3 2.040(4) . ?
Fe1 C3 2.040(4) 7_556 ?
Fe1 C5 2.048(3) 7_556 ?
Fe1 C5 2.048(4) . ?
C1 C2 1.422(5) . ?
C1 C5 1.436(5) . ?
C1 S1 1.760(3) . ?
C2 C3 1.413(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.421(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.500(6) . ?
C6 O7 1.409(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O7 H7 0.77(8) . ?
S1 O8 1.492(3) . ?
S1 C9 1.849(4) . ?
C9 C12 1.518(6) . ?
C9 C11 1.519(5) . ?
C9 C10 1.524(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
C1 Fe1 C1 154.57(19) 7_556 . ?
C1 Fe1 C2 41.15(13) 7_556 7_556 ?
C1 Fe1 C2 163.62(14) . 7_556 ?
C1 Fe1 C2 163.62(14) 7_556 . ?
C1 Fe1 C2 41.15(13) . . ?
C2 Fe1 C2 124.1(2) 7_556 . ?
C1 Fe1 C4 68.05(14) 7_556 7_556 ?
C1 Fe1 C4 109.78(14) . 7_556 ?
C2 Fe1 C4 68.00(18) 7_556 7_556 ?
C2 Fe1 C4 116.75(18) . 7_556 ?
C1 Fe1 C4 109.78(14) 7_556 . ?
C1 Fe1 C4 68.05(14) . . ?
C2 Fe1 C4 116.75(19) 7_556 . ?
C2 Fe1 C4 68.00(18) . . ?
C4 Fe1 C4 170.8(3) 7_556 . ?
C1 Fe1 C3 127.31(15) 7_556 . ?
C1 Fe1 C3 68.36(16) . . ?
C2 Fe1 C3 104.66(19) 7_556 . ?
C2 Fe1 C3 40.67(17) . . ?
C4 Fe1 C3 148.7(2) 7_556 . ?
C4 Fe1 C3 39.83(19) . . ?
C1 Fe1 C3 68.36(16) 7_556 7_556 ?
C1 Fe1 C3 127.31(15) . 7_556 ?
C2 Fe1 C3 40.67(17) 7_556 7_556 ?
C2 Fe1 C3 104.66(19) . 7_556 ?
C4 Fe1 C3 39.83(19) 7_556 7_556 ?
C4 Fe1 C3 148.7(2) . 7_556 ?
C3 Fe1 C3 114.8(3) . 7_556 ?
C1 Fe1 C5 41.34(13) 7_556 7_556 ?
C1 Fe1 C5 120.04(14) . 7_556 ?
C2 Fe1 C5 69.66(16) 7_556 7_556 ?
C2 Fe1 C5 151.70(15) . 7_556 ?
C4 Fe1 C5 40.73(17) 7_556 7_556 ?
C4 Fe1 C5 131.79(19) . 7_556 ?
C3 Fe1 C5 167.50(17) . 7_556 ?
C3 Fe1 C5 68.7(2) 7_556 7_556 ?
C1 Fe1 C5 120.04(14) 7_556 . ?
C1 Fe1 C5 41.34(13) . . ?
C2 Fe1 C5 151.70(15) 7_556 . ?
C2 Fe1 C5 69.66(16) . . ?
C4 Fe1 C5 131.79(19) 7_556 . ?
C4 Fe1 C5 40.73(17) . . ?
C3 Fe1 C5 68.7(2) . . ?
C3 Fe1 C5 167.50(17) 7_556 . ?
C5 Fe1 C5 110.7(2) 7_556 . ?
C2 C1 C5 109.0(3) . . ?
C2 C1 S1 120.4(3) . . ?
C5 C1 S1 130.4(3) . . ?
C2 C1 Fe1 69.68(19) . . ?
C5 C1 Fe1 70.35(18) . . ?
S1 C1 Fe1 121.65(16) . . ?
C3 C2 C1 107.1(4) . . ?
C3 C2 Fe1 70.1(2) . . ?
C1 C2 Fe1 69.17(18) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
Fe1 C2 H2 125.8 . . ?
C4 C3 C2 108.4(4) . . ?
C4 C3 Fe1 69.9(2) . . ?
C2 C3 Fe1 69.2(2) . . ?
C4 C3 H3 125.8 . . ?
C2 C3 H3 125.8 . . ?
Fe1 C3 H3 126.7 . . ?
C3 C4 C5 110.3(4) . . ?
C3 C4 Fe1 70.3(2) . . ?
C5 C4 Fe1 70.10(19) . . ?
C3 C4 H4 124.8 . . ?
C5 C4 H4 124.8 . . ?
Fe1 C4 H4 126.4 . . ?
C4 C5 C1 105.2(4) . . ?
C4 C5 C6 125.7(4) . . ?
C1 C5 C6 129.0(4) . . ?
C4 C5 Fe1 69.2(2) . . ?
C1 C5 Fe1 68.31(19) . . ?
C6 C5 Fe1 128.9(3) . . ?
O7 C6 C5 111.0(5) . . ?
O7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
O7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 O7 H7 110(5) . . ?
O8 S1 C1 106.98(17) . . ?
O8 S1 C9 105.7(2) . . ?
C1 S1 C9 102.79(16) . . ?
C12 C9 C11 111.0(4) . . ?
C12 C9 C10 111.9(4) . . ?
C11 C9 C10 112.2(4) . . ?
C12 C9 S1 107.0(3) . . ?
C11 C9 S1 103.8(3) . . ?
C10 C9 S1 110.4(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job_H7.res
#...............................................................................


####################################################################### 
# 
# 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_MW856_2
_database_code_depnum_ccdc_archive 'CCDC 2236043'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;Institut des Sciences Chimiques de Rennes
France
;
_audit_update_record             
;
2023-01-13 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 13 decembre 2022                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H24 F2 Fe O2 S2'
_chemical_formula_sum            'C18 H24 F2 Fe O2 S2'
_chemical_formula_weight         430.34
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'
_space_group_IT_number           5
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.4422(19)
_cell_length_b                   10.1230(10)
_cell_length_c                   6.0952(7)
_cell_angle_alpha                90
_cell_angle_beta                 101.428(4)
_cell_angle_gamma                90
_cell_volume                     1115.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8936
_cell_measurement_theta_min      2.2531
_cell_measurement_theta_max      27.4302
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0551153
_diffrn_orient_matrix_UB_21      -0.0002863
_diffrn_orient_matrix_UB_31      0.0046920
_diffrn_orient_matrix_UB_12      -0.0081691
_diffrn_orient_matrix_UB_22      0.0169373
_diffrn_orient_matrix_UB_32      0.0969930
_diffrn_orient_matrix_UB_13      0.0297669
_diffrn_orient_matrix_UB_23      -0.1617127
_diffrn_orient_matrix_UB_33      0.0307460


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.050
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             448
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_T_max  0.957

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2022.1-1        #
# Number of scans            :        4                                        #
# Total number of frames [*] :      554                                        #
# Total length of scans  [*] :   554.00 (deg.)                                 #
# Rotation speed         [*] :    10.00 sec./deg.                              #
# Total exposition time  [*] :      1 h    32 min.                             #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     1.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Omega   10.0  1.00    34.0    97   97.0    0.1    2.7    0.0  -44.5 150.0 #
#  3 Omega   10.0  1.00    34.0    97   97.0    0.1   99.7  144.0  -44.5 150.0 #
#  4 Phi     10.0  1.00    34.0   360  360.0    0.1  270.3  360.0   24.0 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0249
_diffrn_reflns_av_r_equivalents  0.0322
_diffrn_reflns_number            11881
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         2.306
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             2355
_reflns_number_gt                2321
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_max     0.826
_reflns_Friedel_fraction_full    0.869

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019_2 (Sheldrick, 2019)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²+1.5337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2355
_refine_ls_number_parameters     117
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 
;
Flack x determined using 979 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(8)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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'

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 0.56871(17) 0.6667(4) 0.3055(6) 0.0211(7) Uani 1 1 d . . . . .
H1 H 0.555256 0.607238 0.183669 0.025 Uiso 1 1 calc R U . . .
C2 C 0.5672(2) 0.8065(4) 0.2913(6) 0.0259(8) Uani 1 1 d . . . . .
H2 H 0.552559 0.856338 0.157835 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5911(2) 0.8599(4) 0.5096(7) 0.0252(8) Uani 1 1 d . . . . .
H3 H 0.594965 0.950805 0.549142 0.030 Uiso 1 1 calc R U . . .
C4 C 0.60798(15) 0.7508(4) 0.6559(5) 0.0208(6) Uani 1 1 d . . . . .
C5 C 0.59400(18) 0.6308(4) 0.5347(6) 0.0192(7) Uani 1 1 d . . . . .
F6 F 0.63548(10) 0.7615(2) 0.8762(3) 0.0306(5) Uani 1 1 d . . . . .
O7 O 0.59043(15) 0.4712(3) 0.8737(4) 0.0326(6) Uani 1 1 d . . . . .
C8 C 0.69653(18) 0.4250(4) 0.6346(6) 0.0264(7) Uani 1 1 d . . . . .
C9 C 0.7053(2) 0.4305(4) 0.3894(6) 0.0334(9) Uani 1 1 d . . . . .
H9A H 0.701958 0.522372 0.337900 0.050 Uiso 1 1 calc R U . . .
H9B H 0.666024 0.378379 0.296658 0.050 Uiso 1 1 calc R U . . .
H9C H 0.753611 0.394078 0.377152 0.050 Uiso 1 1 calc R U . . .
C10 C 0.7061(2) 0.2866(5) 0.7278(8) 0.0411(10) Uani 1 1 d . . . . .
H10A H 0.671937 0.226882 0.631317 0.062 Uiso 1 1 calc R U . . .
H10B H 0.695372 0.285581 0.879036 0.062 Uiso 1 1 calc R U . . .
H10C H 0.757070 0.257328 0.733670 0.062 Uiso 1 1 calc R U . . .
C11 C 0.7476(2) 0.5216(5) 0.7818(7) 0.0350(9) Uani 1 1 d . . . . .
H11A H 0.798568 0.488652 0.806039 0.053 Uiso 1 1 calc R U . . .
H11B H 0.732348 0.530408 0.926210 0.053 Uiso 1 1 calc R U . . .
H11C H 0.744916 0.607991 0.708037 0.053 Uiso 1 1 calc R U . . .
Fe1 Fe 0.500000 0.74115(4) 0.500000 0.01634(16) Uani 1 2 d S T P . .
S1 S 0.59828(4) 0.46565(9) 0.63474(13) 0.02211(19) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C2 1.417(5) . ?
C1 C5 1.430(5) . ?
C1 Fe1 2.043(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.423(6) . ?
C2 Fe1 2.053(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.415(5) . ?
C3 Fe1 2.057(4) . ?
C3 H3 0.9500 . ?
C4 F6 1.342(3) . ?
C4 C5 1.419(5) . ?
C4 Fe1 2.032(3) . ?
C5 S1 1.776(4) . ?
C5 Fe1 2.038(3) . ?
O7 S1 1.493(3) . ?
C8 C10 1.510(6) . ?
C8 C11 1.521(5) . ?
C8 C9 1.536(5) . ?
C8 S1 1.858(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

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
C2 C1 C5 108.2(3) . . ?
C2 C1 Fe1 70.1(2) . . ?
C5 C1 Fe1 69.30(19) . . ?
C2 C1 H1 125.9 . . ?
C5 C1 H1 125.9 . . ?
Fe1 C1 H1 126.2 . . ?
C1 C2 C3 108.9(4) . . ?
C1 C2 Fe1 69.4(2) . . ?
C3 C2 Fe1 69.9(2) . . ?
C1 C2 H2 125.5 . . ?
C3 C2 H2 125.5 . . ?
Fe1 C2 H2 126.7 . . ?
C4 C3 C2 106.3(4) . . ?
C4 C3 Fe1 68.78(19) . . ?
C2 C3 Fe1 69.6(2) . . ?
C4 C3 H3 126.8 . . ?
C2 C3 H3 126.8 . . ?
Fe1 C3 H3 126.4 . . ?
F6 C4 C3 124.1(4) . . ?
F6 C4 C5 125.7(3) . . ?
C3 C4 C5 110.2(3) . . ?
F6 C4 Fe1 127.79(19) . . ?
C3 C4 Fe1 70.73(19) . . ?
C5 C4 Fe1 69.82(18) . . ?
C4 C5 C1 106.3(3) . . ?
C4 C5 S1 129.5(3) . . ?
C1 C5 S1 124.0(3) . . ?
C4 C5 Fe1 69.36(18) . . ?
C1 C5 Fe1 69.69(19) . . ?
S1 C5 Fe1 122.06(17) . . ?
C10 C8 C11 111.2(3) . . ?
C10 C8 C9 111.9(3) . . ?
C11 C8 C9 112.2(3) . . ?
C10 C8 S1 104.2(3) . . ?
C11 C8 S1 110.3(3) . . ?
C9 C8 S1 106.5(2) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C4 Fe1 C4 174.5(2) . 2_656 ?
C4 Fe1 C5 144.06(15) . 2_656 ?
C4 Fe1 C5 40.81(15) 2_656 2_656 ?
C4 Fe1 C5 40.81(15) . . ?
C4 Fe1 C5 144.06(15) 2_656 . ?
C5 Fe1 C5 113.5(2) 2_656 . ?
C4 Fe1 C1 68.04(13) . . ?
C4 Fe1 C1 114.16(13) 2_656 . ?
C5 Fe1 C1 110.50(14) 2_656 . ?
C5 Fe1 C1 41.01(13) . . ?
C4 Fe1 C1 114.16(13) . 2_656 ?
C4 Fe1 C1 68.05(13) 2_656 2_656 ?
C5 Fe1 C1 41.01(13) 2_656 2_656 ?
C5 Fe1 C1 110.50(14) . 2_656 ?
C1 Fe1 C1 136.7(2) . 2_656 ?
C4 Fe1 C2 110.52(13) . 2_656 ?
C4 Fe1 C2 67.57(13) 2_656 2_656 ?
C5 Fe1 C2 68.63(15) 2_656 2_656 ?
C5 Fe1 C2 135.86(14) . 2_656 ?
C1 Fe1 C2 176.50(17) . 2_656 ?
C1 Fe1 C2 40.48(13) 2_656 2_656 ?
C4 Fe1 C2 67.57(13) . . ?
C4 Fe1 C2 110.52(13) 2_656 . ?
C5 Fe1 C2 135.86(14) 2_656 . ?
C5 Fe1 C2 68.63(15) . . ?
C1 Fe1 C2 40.48(13) . . ?
C1 Fe1 C2 176.50(17) 2_656 . ?
C2 Fe1 C2 142.4(2) 2_656 . ?
C4 Fe1 C3 134.77(15) . 2_656 ?
C4 Fe1 C3 40.49(15) 2_656 2_656 ?
C5 Fe1 C3 69.18(13) 2_656 2_656 ?
C5 Fe1 C3 175.16(16) . 2_656 ?
C1 Fe1 C3 142.74(15) . 2_656 ?
C1 Fe1 C3 68.60(15) 2_656 2_656 ?
C2 Fe1 C3 40.50(16) 2_656 2_656 ?
C2 Fe1 C3 112.57(16) . 2_656 ?
C4 Fe1 C3 40.49(15) . . ?
C4 Fe1 C3 134.77(15) 2_656 . ?
C5 Fe1 C3 175.16(16) 2_656 . ?
C5 Fe1 C3 69.18(13) . . ?
C1 Fe1 C3 68.60(15) . . ?
C1 Fe1 C3 142.74(15) 2_656 . ?
C2 Fe1 C3 112.57(16) 2_656 . ?
C2 Fe1 C3 40.50(16) . . ?
C3 Fe1 C3 108.5(2) 2_656 . ?
O7 S1 C5 107.04(16) . . ?
O7 S1 C8 106.97(16) . . ?
C5 S1 C8 100.67(17) . . ?

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
C5 C1 C2 C3 -0.1(4) . . . . ?
Fe1 C1 C2 C3 58.9(3) . . . . ?
C5 C1 C2 Fe1 -59.0(2) . . . . ?
C1 C2 C3 C4 0.7(4) . . . . ?
Fe1 C2 C3 C4 59.2(2) . . . . ?
C1 C2 C3 Fe1 -58.6(3) . . . . ?
C2 C3 C4 F6 177.1(3) . . . . ?
Fe1 C3 C4 F6 -123.2(3) . . . . ?
C2 C3 C4 C5 -1.0(3) . . . . ?
Fe1 C3 C4 C5 58.8(2) . . . . ?
C2 C3 C4 Fe1 -59.7(2) . . . . ?
F6 C4 C5 C1 -177.1(3) . . . . ?
C3 C4 C5 C1 0.9(3) . . . . ?
Fe1 C4 C5 C1 60.2(2) . . . . ?
F6 C4 C5 S1 7.5(5) . . . . ?
C3 C4 C5 S1 -174.5(3) . . . . ?
Fe1 C4 C5 S1 -115.1(3) . . . . ?
F6 C4 C5 Fe1 122.7(3) . . . . ?
C3 C4 C5 Fe1 -59.3(2) . . . . ?
C2 C1 C5 C4 -0.4(4) . . . . ?
Fe1 C1 C5 C4 -60.0(2) . . . . ?
C2 C1 C5 S1 175.2(3) . . . . ?
Fe1 C1 C5 S1 115.7(2) . . . . ?
C2 C1 C5 Fe1 59.5(3) . . . . ?
C4 C5 S1 O7 22.0(3) . . . . ?
C1 C5 S1 O7 -152.6(3) . . . . ?
Fe1 C5 S1 O7 -66.7(2) . . . . ?
C4 C5 S1 C8 -89.7(3) . . . . ?
C1 C5 S1 C8 95.7(3) . . . . ?
Fe1 C5 S1 C8 -178.36(19) . . . . ?
C10 C8 S1 O7 66.0(3) . . . . ?
C11 C8 S1 O7 -53.5(3) . . . . ?
C9 C8 S1 O7 -175.6(3) . . . . ?
C10 C8 S1 C5 177.7(3) . . . . ?
C11 C8 S1 C5 58.1(3) . . . . ?
C9 C8 S1 C5 -63.9(3) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: sqz.res
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .FAB SHELXL file: sqz.fab
#...............................................................................



# ............... End of .FAB file ........................................... #
#------------------------------------------------------------------------------#

#------------------------------------------------------------------------------#
#===END OF CIF FILE FOR MW856_2                                                #
#------------------------------------------------------------------------------#
#                                                                              #
################################################################################
####################################################################### 
# 
# 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_MW525
_database_code_depnum_ccdc_archive 'CCDC 2204523'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-30 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 10 juin 2022                                             #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H40 F2 Fe O2 S2 Si2'
_chemical_formula_sum            'C24 H40 F2 Fe O2 S2 Si2'
_chemical_formula_weight         574.71
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 43'
_space_group_name_Hall           'P 4cw'
_space_group_IT_number           78
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+3/4'
'y, -x, z+1/4'

_cell_length_a                   12.9086(13)
_cell_length_b                   12.9086
_cell_length_c                   17.950(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2991.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.5033
_cell_measurement_theta_max      26.9734
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0556878
_diffrn_orient_matrix_UB_21      -0.0510969
_diffrn_orient_matrix_UB_31      -0.0170061
_diffrn_orient_matrix_UB_12      -0.0125201
_diffrn_orient_matrix_UB_22      0.0115089
_diffrn_orient_matrix_UB_32      -0.0755779
_diffrn_orient_matrix_UB_13      0.0376668
_diffrn_orient_matrix_UB_23      0.0410475
_diffrn_orient_matrix_UB_33      0.0000109


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1216
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_T_max  0.913

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2021.10-0       #
# Number of scans            :        3                                        #
# Total number of frames [*] :      248                                        #
# Total length of scans  [*] :   248.00 (deg.)                                 #
# Rotation speed         [*] :     5.00 sec./deg.                              #
# Total exposition time  [*] :         20.7 min.                               #
#                                                                              #
#  [*] fast scan not included                                                  #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Fast     1.0  1.00    34.0   180  180.0    0.0    0.0    0.0   54.7 150.0 #
#  2 Omega    5.0  1.00    34.0    97   97.0    0.1    2.7   72.0  -44.5 150.0 #
#  3 Phi      5.0  1.00    34.0   151  151.0    0.1  270.3  288.5   24.0 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0448
_diffrn_reflns_av_r_equivalents  0.0516
_diffrn_reflns_number            28620
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.943
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             6869
_reflns_number_gt                6469
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.998

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0240P)²+0.3712P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6869
_refine_ls_number_parameters     310
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0631
_refine_ls_wR_factor_gt          0.0612
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 
;
Flack x determined using 2905 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(8)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.45275(3) 0.17608(3) 0.44398(2) 0.01674(9) Uani 1 1 d . . . . .
C1 C 0.30371(19) 0.1156(2) 0.42760(15) 0.0192(5) Uani 1 1 d . . . . .
C2 C 0.3593(2) 0.1290(2) 0.35857(16) 0.0211(5) Uani 1 1 d . . . . .
H2 H 0.373894 0.075372 0.323891 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3892(2) 0.2345(2) 0.35012(15) 0.0204(5) Uani 1 1 d . . . . .
H3 H 0.426789 0.262858 0.309468 0.024 Uiso 1 1 calc R U . . .
C4 C 0.3524(2) 0.2903(2) 0.41380(14) 0.0180(5) Uani 1 1 d . . . . .
C5 C 0.30124(19) 0.2164(2) 0.45916(14) 0.0183(5) Uani 1 1 d . . . . .
F6 F 0.25067(12) 0.23931(12) 0.52261(9) 0.0238(3) Uani 1 1 d . . . . .
C7 C 0.2537(2) -0.0265(2) 0.55977(18) 0.0311(7) Uani 1 1 d . . . . .
H7A H 0.327829 -0.032406 0.570718 0.047 Uiso 1 1 calc R U . . .
H7B H 0.218512 -0.090653 0.574436 0.047 Uiso 1 1 calc R U . . .
H7C H 0.224430 0.031809 0.587653 0.047 Uiso 1 1 calc R U . . .
Si1 Si 0.23535(6) -0.00458(6) 0.45881(5) 0.02205(16) Uani 1 1 d . . . . .
C8 C 0.0943(2) 0.0139(3) 0.4397(2) 0.0400(8) Uani 1 1 d . . . . .
H8A H 0.055335 -0.044989 0.459736 0.060 Uiso 1 1 calc R U . . .
H8B H 0.083017 0.018615 0.385842 0.060 Uiso 1 1 calc R U . . .
H8C H 0.070472 0.077940 0.463606 0.060 Uiso 1 1 calc R U . . .
C9 C 0.2848(3) -0.1153(2) 0.4035(2) 0.0346(7) Uani 1 1 d . . . . .
H9A H 0.360306 -0.119200 0.408391 0.052 Uiso 1 1 calc R U . . .
H9B H 0.266485 -0.105571 0.350943 0.052 Uiso 1 1 calc R U . . .
H9C H 0.253735 -0.179739 0.421792 0.052 Uiso 1 1 calc R U . . .
S1 S 0.37979(5) 0.42339(5) 0.42769(4) 0.01954(14) Uani 1 1 d . . . . .
O10 O 0.37108(16) 0.44523(16) 0.50914(12) 0.0270(4) Uani 1 1 d . . . . .
C11 C 0.2641(2) 0.4812(2) 0.38269(16) 0.0228(6) Uani 1 1 d . . . . .
C12 C 0.2836(3) 0.5977(2) 0.3869(2) 0.0351(7) Uani 1 1 d . . . . .
H12A H 0.226547 0.634626 0.362453 0.053 Uiso 1 1 calc R U . . .
H12B H 0.348834 0.614273 0.361638 0.053 Uiso 1 1 calc R U . . .
H12C H 0.287793 0.619097 0.439160 0.053 Uiso 1 1 calc R U . . .
C13 C 0.1676(2) 0.4505(2) 0.42590(17) 0.0291(6) Uani 1 1 d . . . . .
H13A H 0.108011 0.489726 0.407194 0.044 Uiso 1 1 calc R U . . .
H13B H 0.177688 0.465702 0.478884 0.044 Uiso 1 1 calc R U . . .
H13C H 0.154746 0.376172 0.419461 0.044 Uiso 1 1 calc R U . . .
C14 C 0.2621(3) 0.4458(2) 0.30183(17) 0.0301(7) Uani 1 1 d . . . . .
H14A H 0.245332 0.371776 0.299721 0.045 Uiso 1 1 calc R U . . .
H14B H 0.330129 0.457585 0.279180 0.045 Uiso 1 1 calc R U . . .
H14C H 0.209431 0.485143 0.274515 0.045 Uiso 1 1 calc R U . . .
C21 C 0.58565(19) 0.0919(2) 0.43415(16) 0.0209(5) Uani 1 1 d . . . . .
C22 C 0.6044(2) 0.1993(2) 0.42203(16) 0.0230(6) Uani 1 1 d . . . . .
H22 H 0.630710 0.229646 0.377660 0.028 Uiso 1 1 calc R U . . .
C23 C 0.5768(2) 0.2530(2) 0.48825(16) 0.0227(6) Uani 1 1 d . . . . .
H23 H 0.582162 0.325784 0.495139 0.027 Uiso 1 1 calc R U . . .
C24 C 0.5395(2) 0.1814(2) 0.54317(16) 0.0215(6) Uani 1 1 d . . . . .
C25 C 0.5455(2) 0.0833(2) 0.50750(15) 0.0204(5) Uani 1 1 d . . . . .
F26 F 0.52184(13) -0.00637(12) 0.54128(10) 0.0269(4) Uani 1 1 d . . . . .
C27 C 0.6133(3) 0.1328(3) 0.6975(2) 0.0438(8) Uani 1 1 d . . . . .
H27A H 0.599250 0.139246 0.750954 0.066 Uiso 1 1 calc R U . . .
H27B H 0.683094 0.158758 0.686796 0.066 Uiso 1 1 calc R U . . .
H27C H 0.608548 0.059856 0.682804 0.066 Uiso 1 1 calc R U . . .
Si2 Si 0.51638(7) 0.21004(7) 0.64414(5) 0.02670(18) Uani 1 1 d . . . . .
C28 C 0.5369(3) 0.3512(3) 0.6572(2) 0.0454(9) Uani 1 1 d . . . . .
H28A H 0.489408 0.389694 0.624806 0.068 Uiso 1 1 calc R U . . .
H28B H 0.608563 0.368874 0.644345 0.068 Uiso 1 1 calc R U . . .
H28C H 0.523612 0.369627 0.709277 0.068 Uiso 1 1 calc R U . . .
C29 C 0.3863(3) 0.1704(3) 0.67683(18) 0.0382(8) Uani 1 1 d . . . . .
H29A H 0.380476 0.094713 0.674761 0.057 Uiso 1 1 calc R U . . .
H29B H 0.333321 0.201526 0.644789 0.057 Uiso 1 1 calc R U . . .
H29C H 0.376235 0.193808 0.728248 0.057 Uiso 1 1 calc R U . . .
S2 S 0.61309(5) -0.00557(6) 0.36732(4) 0.02444(15) Uani 1 1 d . . . . .
O30 O 0.54559(17) -0.09662(18) 0.38198(16) 0.0402(6) Uani 1 1 d . . . . .
C31 C 0.7456(2) -0.0412(2) 0.39886(18) 0.0252(6) Uani 1 1 d . . . . .
C32 C 0.7807(3) -0.1223(3) 0.3428(2) 0.0411(8) Uani 1 1 d . . . . .
H32A H 0.852022 -0.143151 0.354015 0.062 Uiso 1 1 calc R U . . .
H32B H 0.777659 -0.093057 0.292443 0.062 Uiso 1 1 calc R U . . .
H32C H 0.735126 -0.182826 0.345787 0.062 Uiso 1 1 calc R U . . .
C33 C 0.7418(3) -0.0861(3) 0.4763(2) 0.0407(8) Uani 1 1 d . . . . .
H33A H 0.688861 -0.140430 0.478395 0.061 Uiso 1 1 calc R U . . .
H33B H 0.724589 -0.031311 0.512021 0.061 Uiso 1 1 calc R U . . .
H33C H 0.809476 -0.115723 0.488846 0.061 Uiso 1 1 calc R U . . .
C34 C 0.8124(2) 0.0554(3) 0.3935(2) 0.0416(8) Uani 1 1 d . . . . .
H34A H 0.790896 0.105174 0.431756 0.062 Uiso 1 1 calc R U . . .
H34B H 0.804221 0.086620 0.344127 0.062 Uiso 1 1 calc R U . . .
H34C H 0.885175 0.036696 0.401314 0.062 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C3 2.020(3) . ?
Fe1 C22 2.020(3) . ?
Fe1 C4 2.036(3) . ?
Fe1 C21 2.038(3) . ?
Fe1 C5 2.042(2) . ?
Fe1 C25 2.042(3) . ?
Fe1 C2 2.043(3) . ?
Fe1 C23 2.045(3) . ?
Fe1 C1 2.097(3) . ?
Fe1 C24 2.104(3) . ?
C1 C5 1.419(4) . ?
C1 C2 1.442(4) . ?
C1 Si1 1.871(3) . ?
C2 C3 1.423(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.432(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.418(4) . ?
C4 S1 1.772(3) . ?
C5 F6 1.346(3) . ?
C7 Si1 1.849(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
Si1 C9 1.854(3) . ?
Si1 C8 1.868(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
S1 O10 1.493(2) . ?
S1 C11 1.854(3) . ?
C11 C14 1.522(4) . ?
C11 C13 1.521(4) . ?
C11 C12 1.527(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 C25 1.419(4) . ?
C21 C22 1.424(4) . ?
C21 S2 1.774(3) . ?
C22 C23 1.422(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.435(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.421(4) . ?
C24 Si2 1.874(3) . ?
C25 F26 1.342(3) . ?
C27 Si2 1.865(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
Si2 C29 1.851(3) . ?
Si2 C28 1.856(4) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
S2 O30 1.487(2) . ?
S2 C31 1.859(3) . ?
C31 C33 1.507(5) . ?
C31 C34 1.519(4) . ?
C31 C32 1.521(4) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

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
C3 Fe1 C22 100.12(12) . . ?
C3 Fe1 C4 41.34(10) . . ?
C22 Fe1 C4 117.22(11) . . ?
C3 Fe1 C21 117.96(11) . . ?
C22 Fe1 C21 41.09(11) . . ?
C4 Fe1 C21 153.97(11) . . ?
C3 Fe1 C5 68.10(11) . . ?
C22 Fe1 C5 156.45(11) . . ?
C4 Fe1 C5 40.68(10) . . ?
C21 Fe1 C5 162.45(11) . . ?
C3 Fe1 C25 157.39(11) . . ?
C22 Fe1 C25 68.13(11) . . ?
C4 Fe1 C25 161.18(11) . . ?
C21 Fe1 C25 40.71(11) . . ?
C5 Fe1 C25 129.54(10) . . ?
C3 Fe1 C2 41.00(11) . . ?
C22 Fe1 C2 118.04(11) . . ?
C4 Fe1 C2 68.90(11) . . ?
C21 Fe1 C2 105.87(11) . . ?
C5 Fe1 C2 67.08(10) . . ?
C25 Fe1 C2 126.22(11) . . ?
C3 Fe1 C23 117.45(11) . . ?
C22 Fe1 C23 40.94(12) . . ?
C4 Fe1 C23 104.47(11) . . ?
C21 Fe1 C23 68.50(11) . . ?
C5 Fe1 C23 125.05(11) . . ?
C25 Fe1 C23 66.96(11) . . ?
C2 Fe1 C23 153.93(12) . . ?
C3 Fe1 C1 69.46(11) . . ?
C22 Fe1 C1 156.56(11) . . ?
C4 Fe1 C1 69.41(11) . . ?
C21 Fe1 C1 124.18(10) . . ?
C5 Fe1 C1 40.07(10) . . ?
C25 Fe1 C1 113.47(10) . . ?
C2 Fe1 C1 40.75(11) . . ?
C23 Fe1 C1 162.48(11) . . ?
C3 Fe1 C24 155.47(11) . . ?
C22 Fe1 C24 69.18(11) . . ?
C4 Fe1 C24 122.69(11) . . ?
C21 Fe1 C24 69.07(11) . . ?
C5 Fe1 C24 112.85(11) . . ?
C25 Fe1 C24 40.04(11) . . ?
C2 Fe1 C24 163.46(11) . . ?
C23 Fe1 C24 40.44(11) . . ?
C1 Fe1 C24 128.23(11) . . ?
C5 C1 C2 104.1(2) . . ?
C5 C1 Si1 129.0(2) . . ?
C2 C1 Si1 126.3(2) . . ?
C5 C1 Fe1 67.89(14) . . ?
C2 C1 Fe1 67.61(14) . . ?
Si1 C1 Fe1 134.38(14) . . ?
C3 C2 C1 109.9(2) . . ?
C3 C2 Fe1 68.64(15) . . ?
C1 C2 Fe1 71.63(15) . . ?
C3 C2 H2 125.0 . . ?
C1 C2 H2 125.0 . . ?
Fe1 C2 H2 126.3 . . ?
C2 C3 C4 107.8(2) . . ?
C2 C3 Fe1 70.36(15) . . ?
C4 C3 Fe1 69.94(15) . . ?
C2 C3 H3 126.1 . . ?
C4 C3 H3 126.1 . . ?
Fe1 C3 H3 125.2 . . ?
C5 C4 C3 105.9(2) . . ?
C5 C4 S1 131.7(2) . . ?
C3 C4 S1 122.3(2) . . ?
C5 C4 Fe1 69.88(15) . . ?
C3 C4 Fe1 68.72(14) . . ?
S1 C4 Fe1 122.52(14) . . ?
F6 C5 C4 124.3(2) . . ?
F6 C5 C1 123.4(2) . . ?
C4 C5 C1 112.2(2) . . ?
F6 C5 Fe1 129.31(18) . . ?
C4 C5 Fe1 69.44(14) . . ?
C1 C5 Fe1 72.05(15) . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C7 Si1 C9 111.28(16) . . ?
C7 Si1 C8 108.91(17) . . ?
C9 Si1 C8 109.63(17) . . ?
C7 Si1 C1 111.11(14) . . ?
C9 Si1 C1 108.46(14) . . ?
C8 Si1 C1 107.37(14) . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O10 S1 C4 107.81(12) . . ?
O10 S1 C11 106.86(12) . . ?
C4 S1 C11 99.66(12) . . ?
C14 C11 C13 113.2(3) . . ?
C14 C11 C12 110.2(2) . . ?
C13 C11 C12 111.5(3) . . ?
C14 C11 S1 108.0(2) . . ?
C13 C11 S1 109.45(19) . . ?
C12 C11 S1 104.0(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C25 C21 C22 106.3(2) . . ?
C25 C21 S2 130.1(2) . . ?
C22 C21 S2 123.6(2) . . ?
C25 C21 Fe1 69.77(15) . . ?
C22 C21 Fe1 68.75(15) . . ?
S2 C21 Fe1 127.20(15) . . ?
C23 C22 C21 107.7(2) . . ?
C23 C22 Fe1 70.47(15) . . ?
C21 C22 Fe1 70.16(15) . . ?
C23 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
Fe1 C22 H22 124.8 . . ?
C22 C23 C24 110.2(2) . . ?
C22 C23 Fe1 68.59(16) . . ?
C24 C23 Fe1 72.02(16) . . ?
C22 C23 H23 124.9 . . ?
C24 C23 H23 124.9 . . ?
Fe1 C23 H23 126.0 . . ?
C25 C24 C23 104.3(2) . . ?
C25 C24 Si2 128.4(2) . . ?
C23 C24 Si2 126.2(2) . . ?
C25 C24 Fe1 67.60(15) . . ?
C23 C24 Fe1 67.54(16) . . ?
Si2 C24 Fe1 137.75(15) . . ?
F26 C25 C24 123.5(2) . . ?
F26 C25 C21 124.7(2) . . ?
C24 C25 C21 111.6(2) . . ?
F26 C25 Fe1 128.66(19) . . ?
C24 C25 Fe1 72.35(16) . . ?
C21 C25 Fe1 69.52(15) . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 Si2 C28 111.18(18) . . ?
C29 Si2 C27 107.33(17) . . ?
C28 Si2 C27 111.36(18) . . ?
C29 Si2 C24 113.35(14) . . ?
C28 Si2 C24 107.05(15) . . ?
C27 Si2 C24 106.53(16) . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si2 C29 H29A 109.5 . . ?
Si2 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si2 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O30 S2 C21 108.91(14) . . ?
O30 S2 C31 106.84(14) . . ?
C21 S2 C31 98.81(13) . . ?
C33 C31 C34 113.1(3) . . ?
C33 C31 C32 110.8(3) . . ?
C34 C31 C32 110.7(3) . . ?
C33 C31 S2 110.3(2) . . ?
C34 C31 S2 107.5(2) . . ?
C32 C31 S2 104.1(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

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
C5 C1 C2 C3 0.3(3) . . . . ?
Si1 C1 C2 C3 172.4(2) . . . . ?
Fe1 C1 C2 C3 -58.09(19) . . . . ?
C5 C1 C2 Fe1 58.42(17) . . . . ?
Si1 C1 C2 Fe1 -129.5(2) . . . . ?
C1 C2 C3 C4 -0.3(3) . . . . ?
Fe1 C2 C3 C4 -60.16(18) . . . . ?
C1 C2 C3 Fe1 59.89(19) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
Fe1 C3 C4 C5 -60.34(17) . . . . ?
C2 C3 C4 S1 176.30(19) . . . . ?
Fe1 C3 C4 S1 115.87(19) . . . . ?
C2 C3 C4 Fe1 60.43(18) . . . . ?
C3 C4 C5 F6 -176.1(2) . . . . ?
S1 C4 C5 F6 8.1(4) . . . . ?
Fe1 C4 C5 F6 124.3(2) . . . . ?
C3 C4 C5 C1 0.1(3) . . . . ?
S1 C4 C5 C1 -175.6(2) . . . . ?
Fe1 C4 C5 C1 -59.45(19) . . . . ?
C3 C4 C5 Fe1 59.58(17) . . . . ?
S1 C4 C5 Fe1 -116.1(2) . . . . ?
C2 C1 C5 F6 176.0(2) . . . . ?
Si1 C1 C5 F6 4.2(4) . . . . ?
Fe1 C1 C5 F6 -125.7(2) . . . . ?
C2 C1 C5 C4 -0.3(3) . . . . ?
Si1 C1 C5 C4 -172.07(19) . . . . ?
Fe1 C1 C5 C4 57.95(19) . . . . ?
C2 C1 C5 Fe1 -58.24(17) . . . . ?
Si1 C1 C5 Fe1 130.0(2) . . . . ?
C5 C1 Si1 C7 -49.1(3) . . . . ?
C2 C1 Si1 C7 140.8(2) . . . . ?
Fe1 C1 Si1 C7 47.6(2) . . . . ?
C5 C1 Si1 C9 -171.7(3) . . . . ?
C2 C1 Si1 C9 18.2(3) . . . . ?
Fe1 C1 Si1 C9 -75.0(2) . . . . ?
C5 C1 Si1 C8 69.9(3) . . . . ?
C2 C1 Si1 C8 -100.2(3) . . . . ?
Fe1 C1 Si1 C8 166.6(2) . . . . ?
C5 C4 S1 O10 18.6(3) . . . . ?
C3 C4 S1 O10 -156.5(2) . . . . ?
Fe1 C4 S1 O10 -72.58(18) . . . . ?
C5 C4 S1 C11 -92.7(3) . . . . ?
C3 C4 S1 C11 92.2(2) . . . . ?
Fe1 C4 S1 C11 176.09(16) . . . . ?
O10 S1 C11 C14 -171.2(2) . . . . ?
C4 S1 C11 C14 -59.2(2) . . . . ?
O10 S1 C11 C13 -47.6(2) . . . . ?
C4 S1 C11 C13 64.5(2) . . . . ?
O10 S1 C11 C12 71.7(2) . . . . ?
C4 S1 C11 C12 -176.3(2) . . . . ?
C25 C21 C22 C23 0.8(3) . . . . ?
S2 C21 C22 C23 -177.9(2) . . . . ?
Fe1 C21 C22 C23 60.78(19) . . . . ?
C25 C21 C22 Fe1 -60.00(18) . . . . ?
S2 C21 C22 Fe1 121.4(2) . . . . ?
C21 C22 C23 C24 -0.4(3) . . . . ?
Fe1 C22 C23 C24 60.2(2) . . . . ?
C21 C22 C23 Fe1 -60.58(19) . . . . ?
C22 C23 C24 C25 -0.2(3) . . . . ?
Fe1 C23 C24 C25 57.97(18) . . . . ?
C22 C23 C24 Si2 168.2(2) . . . . ?
Fe1 C23 C24 Si2 -133.6(2) . . . . ?
C22 C23 C24 Fe1 -58.13(19) . . . . ?
C23 C24 C25 F26 176.9(2) . . . . ?
Si2 C24 C25 F26 8.9(4) . . . . ?
Fe1 C24 C25 F26 -125.1(3) . . . . ?
C23 C24 C25 C21 0.7(3) . . . . ?
Si2 C24 C25 C21 -167.4(2) . . . . ?
Fe1 C24 C25 C21 58.60(19) . . . . ?
C23 C24 C25 Fe1 -57.93(18) . . . . ?
Si2 C24 C25 Fe1 134.0(2) . . . . ?
C22 C21 C25 F26 -177.1(2) . . . . ?
S2 C21 C25 F26 1.4(4) . . . . ?
Fe1 C21 C25 F26 123.5(3) . . . . ?
C22 C21 C25 C24 -0.9(3) . . . . ?
S2 C21 C25 C24 177.6(2) . . . . ?
Fe1 C21 C25 C24 -60.3(2) . . . . ?
C22 C21 C25 Fe1 59.34(18) . . . . ?
S2 C21 C25 Fe1 -122.1(2) . . . . ?
C25 C24 Si2 C29 -65.4(3) . . . . ?
C23 C24 Si2 C29 129.0(3) . . . . ?
Fe1 C24 Si2 C29 33.2(3) . . . . ?
C25 C24 Si2 C28 171.7(3) . . . . ?
C23 C24 Si2 C28 6.1(3) . . . . ?
Fe1 C24 Si2 C28 -89.8(3) . . . . ?
C25 C24 Si2 C27 52.4(3) . . . . ?
C23 C24 Si2 C27 -113.2(3) . . . . ?
Fe1 C24 Si2 C27 151.0(2) . . . . ?
C25 C21 S2 O30 26.2(3) . . . . ?
C22 C21 S2 O30 -155.5(2) . . . . ?
Fe1 C21 S2 O30 -67.9(2) . . . . ?
C25 C21 S2 C31 -85.1(3) . . . . ?
C22 C21 S2 C31 93.2(3) . . . . ?
Fe1 C21 S2 C31 -179.21(18) . . . . ?
O30 S2 C31 C33 -49.2(3) . . . . ?
C21 S2 C31 C33 63.7(2) . . . . ?
O30 S2 C31 C34 -172.9(2) . . . . ?
C21 S2 C31 C34 -59.9(3) . . . . ?
O30 S2 C31 C32 69.7(2) . . . . ?
C21 S2 C31 C32 -177.4(2) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_MW5861
_database_code_depnum_ccdc_archive 'CCDC 2204521'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-30 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 22 fevrier 2022                                          #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C34 H58 Fe O6 S2 Si2, C H Cl3'
_chemical_formula_sum            'C35 H59 Cl3 Fe O6 S2 Si2'
_chemical_formula_weight         858.32
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'
_space_group_IT_number           4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.7592(16)
_cell_length_b                   20.291(3)
_cell_length_c                   10.9077(15)
_cell_angle_alpha                90
_cell_angle_beta                 111.313(4)
_cell_angle_gamma                90
_cell_volume                     2218.4(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3650
_cell_measurement_theta_min      2.2765
_cell_measurement_theta_max      24.8068
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0584914
_diffrn_orient_matrix_UB_21      -0.0807920
_diffrn_orient_matrix_UB_31      0.0021210
_diffrn_orient_matrix_UB_12      -0.0315616
_diffrn_orient_matrix_UB_22      -0.0236244
_diffrn_orient_matrix_UB_32      -0.0295087
_diffrn_orient_matrix_UB_13      0.0663871
_diffrn_orient_matrix_UB_23      0.0019755
_diffrn_orient_matrix_UB_33      -0.0725870


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.530
_exptl_crystal_size_min          0.420
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             908
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_T_max  0.743

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS 2014.5.0.0/23-May-2014 && APEX2_2014.11-0   #
# Number of scans            :        3                                        #
# Total number of frames     :      255                                        #
# Total length of scans      :   255.00 (deg.)                                 #
# Rotation speed             :     5.00 sec./deg.                              #
# Total exposition time      :         21.2 min.                               #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Omega    5.0  1.00    35.0    93   93.0  344.0  343.4   27.6  -28.7 150.0 #
#  2 Omega    5.0  1.00    35.0    94   94.0  344.0  253.5    2.1   25.2 150.0 #
#  3 Omega    5.0  1.00    35.0    68   68.0  344.0  342.5  133.3  -48.1 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_detector_area_resol_mean 8.33
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0765
_diffrn_reflns_av_r_equivalents  0.0271
_diffrn_reflns_number            12799
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.004
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_reflns_number_total             8989
_reflns_number_gt                7236
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_max     0.784
_reflns_Friedel_fraction_full    0.856

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8989
_refine_ls_number_parameters     458
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1344
_refine_ls_wR_factor_gt          0.1222
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 
;
Flack x determined using 2560 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(13)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.53030(7) 0.43631(4) 0.70451(7) 0.01569(18) Uani 1 1 d . . . . .
C1 C 0.4510(6) 0.3791(3) 0.8185(6) 0.0190(14) Uani 1 1 d . . . . .
C2 C 0.3497(6) 0.4079(3) 0.7065(6) 0.0176(13) Uani 1 1 d . . . . .
H2 H 0.284821 0.383474 0.638874 0.021 Uiso 1 1 calc R U . . .
C3 C 0.3591(6) 0.4774(3) 0.7099(6) 0.0205(14) Uani 1 1 d . . . . .
C4 C 0.4706(6) 0.4951(3) 0.8253(6) 0.0192(13) Uani 1 1 d . . . . .
H4 H 0.502376 0.538434 0.852094 0.023 Uiso 1 1 calc R U . . .
C5 C 0.5251(5) 0.4352(4) 0.8925(5) 0.0203(11) Uani 1 1 d . . . . .
Si1 Si 0.45815(19) 0.28746(9) 0.84814(17) 0.0267(4) Uani 1 1 d . . . . .
C6 C 0.3227(7) 0.2521(3) 0.7030(7) 0.0354(16) Uani 1 1 d . . . . .
H6A H 0.320183 0.204158 0.712923 0.053 Uiso 1 1 calc R U . . .
H6B H 0.339721 0.262485 0.622818 0.053 Uiso 1 1 calc R U . . .
H6C H 0.236856 0.271013 0.697019 0.053 Uiso 1 1 calc R U . . .
C7 C 0.6163(8) 0.2465(4) 0.8561(8) 0.0408(18) Uani 1 1 d . . . . .
H7A H 0.692612 0.272934 0.910684 0.061 Uiso 1 1 calc R U . . .
H7B H 0.617873 0.242678 0.767094 0.061 Uiso 1 1 calc R U . . .
H7C H 0.621396 0.202528 0.894597 0.061 Uiso 1 1 calc R U . . .
C8 C 0.4182(8) 0.2686(4) 0.9967(7) 0.0431(19) Uani 1 1 d . . . . .
H8A H 0.397943 0.221611 0.997787 0.065 Uiso 1 1 calc R U . . .
H8B H 0.340679 0.294641 0.994589 0.065 Uiso 1 1 calc R U . . .
H8C H 0.494902 0.279778 1.075893 0.065 Uiso 1 1 calc R U . . .
O9 O 0.6983(5) 0.3620(2) 1.0694(4) 0.0351(11) Uani 1 1 d . . . . .
S1 S 0.67095(13) 0.43259(9) 1.03779(13) 0.0245(3) Uani 1 1 d . . . . .
C10 C 0.6058(7) 0.4670(4) 1.1610(6) 0.0329(16) Uani 1 1 d . . . . .
C11 C 0.4868(7) 0.4274(6) 1.1625(6) 0.056(3) Uani 1 1 d . . . . .
H11A H 0.465969 0.439662 1.239797 0.085 Uiso 1 1 calc R U . . .
H11B H 0.508017 0.380316 1.166299 0.085 Uiso 1 1 calc R U . . .
H11C H 0.409689 0.436691 1.082432 0.085 Uiso 1 1 calc R U . . .
C12 C 0.7234(7) 0.4596(4) 1.2910(6) 0.044(2) Uani 1 1 d . . . . .
H12A H 0.801493 0.482300 1.285113 0.066 Uiso 1 1 calc R U . . .
H12B H 0.743978 0.412766 1.309227 0.066 Uiso 1 1 calc R U . . .
H12C H 0.700375 0.479059 1.362242 0.066 Uiso 1 1 calc R U . . .
C13 C 0.5742(11) 0.5382(5) 1.1295(8) 0.061(3) Uani 1 1 d . . . . .
H13A H 0.483417 0.542401 1.064518 0.091 Uiso 1 1 calc R U . . .
H13B H 0.637708 0.556974 1.093593 0.091 Uiso 1 1 calc R U . . .
H13C H 0.580708 0.561963 1.209890 0.091 Uiso 1 1 calc R U . . .
C14 C 0.2711(6) 0.5221(3) 0.6099(6) 0.0247(14) Uani 1 1 d . . . . .
O15 O 0.1902(5) 0.5043(2) 0.5073(4) 0.0382(12) Uani 1 1 d . . . . .
O16 O 0.2903(4) 0.5849(2) 0.6503(4) 0.0305(10) Uani 1 1 d . . . . .
C17 C 0.2041(7) 0.6328(3) 0.5610(7) 0.0369(17) Uani 1 1 d . . . . .
H17A H 0.109903 0.624143 0.549146 0.044 Uiso 1 1 calc R U . . .
H17B H 0.213098 0.629969 0.474017 0.044 Uiso 1 1 calc R U . . .
C18 C 0.2447(8) 0.7002(4) 0.6193(8) 0.048(2) Uani 1 1 d . . . . .
H18 H 0.341677 0.706775 0.636150 0.057 Uiso 1 1 calc R U . . .
C19 C 0.2228(10) 0.7061(5) 0.7489(9) 0.065(3) Uani 1 1 d . . . . .
H19A H 0.127102 0.704079 0.732392 0.098 Uiso 1 1 calc R U . . .
H19B H 0.258821 0.748247 0.790764 0.098 Uiso 1 1 calc R U . . .
H19C H 0.268517 0.669830 0.807166 0.098 Uiso 1 1 calc R U . . .
C20 C 0.1632(10) 0.7519(5) 0.5168(11) 0.072(3) Uani 1 1 d . . . . .
H20A H 0.168889 0.741996 0.431074 0.109 Uiso 1 1 calc R U . . .
H20B H 0.199473 0.795999 0.545207 0.109 Uiso 1 1 calc R U . . .
H20C H 0.069685 0.750428 0.509390 0.109 Uiso 1 1 calc R U . . .
C21 C 0.7224(5) 0.4443(3) 0.7073(5) 0.0229(13) Uani 1 1 d . . . . .
C22 C 0.6682(6) 0.3813(3) 0.6625(6) 0.0197(13) Uani 1 1 d . . . . .
H22 H 0.702503 0.340161 0.702062 0.024 Uiso 1 1 calc R U . . .
C23 C 0.5520(6) 0.3910(3) 0.5464(6) 0.0187(13) Uani 1 1 d . . . . .
C24 C 0.5343(6) 0.4600(3) 0.5240(6) 0.0185(13) Uani 1 1 d . . . . .
H24 H 0.462937 0.480001 0.454785 0.022 Uiso 1 1 calc R U . . .
C25 C 0.6417(6) 0.4954(3) 0.6230(6) 0.0196(13) Uani 1 1 d . . . . .
Si2 Si 0.6532(2) 0.58814(9) 0.61936(18) 0.0279(4) Uani 1 1 d . . . . .
C26 C 0.8058(8) 0.6155(4) 0.5908(8) 0.044(2) Uani 1 1 d . . . . .
H26A H 0.882960 0.612713 0.673391 0.066 Uiso 1 1 calc R U . . .
H26B H 0.794247 0.661161 0.559383 0.066 Uiso 1 1 calc R U . . .
H26C H 0.820306 0.587032 0.524720 0.066 Uiso 1 1 calc R U . . .
C27 C 0.5066(8) 0.6130(3) 0.4703(7) 0.0388(18) Uani 1 1 d . . . . .
H27A H 0.502726 0.661144 0.463465 0.058 Uiso 1 1 calc R U . . .
H27B H 0.424322 0.596438 0.478326 0.058 Uiso 1 1 calc R U . . .
H27C H 0.516266 0.594313 0.391409 0.058 Uiso 1 1 calc R U . . .
C28 C 0.6406(8) 0.6320(3) 0.7666(7) 0.0392(18) Uani 1 1 d . . . . .
H28A H 0.695499 0.609001 0.847111 0.059 Uiso 1 1 calc R U . . .
H28B H 0.547443 0.632317 0.760359 0.059 Uiso 1 1 calc R U . . .
H28C H 0.672385 0.677380 0.768867 0.059 Uiso 1 1 calc R U . . .
O29 O 0.8768(5) 0.5318(3) 0.8614(4) 0.0373(12) Uani 1 1 d . . . . .
S2 S 0.86666(15) 0.45830(9) 0.84912(15) 0.0285(4) Uani 1 1 d . . . . .
C30 C 0.9989(6) 0.4294(5) 0.7889(6) 0.0356(17) Uani 1 1 d . . . . .
C31 C 1.1263(7) 0.4580(6) 0.8922(8) 0.064(3) Uani 1 1 d . . . . .
H31A H 1.130536 0.445609 0.980480 0.096 Uiso 1 1 calc R U . . .
H31B H 1.125075 0.506179 0.884687 0.096 Uiso 1 1 calc R U . . .
H31C H 1.204634 0.440560 0.877427 0.096 Uiso 1 1 calc R U . . .
C32 C 1.0009(9) 0.3565(5) 0.7923(10) 0.063(3) Uani 1 1 d . . . . .
H32A H 0.919945 0.339431 0.724137 0.094 Uiso 1 1 calc R U . . .
H32B H 1.004435 0.341349 0.878866 0.094 Uiso 1 1 calc R U . . .
H32C H 1.079498 0.340432 0.776298 0.094 Uiso 1 1 calc R U . . .
C33 C 0.9788(7) 0.4563(5) 0.6529(7) 0.050(2) Uani 1 1 d . . . . .
H33A H 1.049392 0.439465 0.624431 0.075 Uiso 1 1 calc R U . . .
H33B H 0.982475 0.504508 0.656154 0.075 Uiso 1 1 calc R U . . .
H33C H 0.891732 0.442102 0.590528 0.075 Uiso 1 1 calc R U . . .
C34 C 0.4671(6) 0.3372(3) 0.4688(6) 0.0225(13) Uani 1 1 d . . . . .
O35 O 0.5002(5) 0.2802(2) 0.4803(5) 0.0378(12) Uani 1 1 d . . . . .
O36 O 0.3518(4) 0.3595(2) 0.3826(4) 0.0259(10) Uani 1 1 d . . . . .
C37 C 0.2653(6) 0.3100(3) 0.2982(7) 0.0293(15) Uani 1 1 d . . . . .
H37A H 0.258421 0.271685 0.351606 0.035 Uiso 1 1 calc R U . . .
H37B H 0.303020 0.294582 0.232900 0.035 Uiso 1 1 calc R U . . .
C38 C 0.1317(7) 0.3386(4) 0.2298(7) 0.0377(17) Uani 1 1 d . . . . .
H38 H 0.140236 0.378193 0.178836 0.045 Uiso 1 1 calc R U . . .
C39 C 0.0446(8) 0.2863(5) 0.1333(8) 0.052(2) Uani 1 1 d . . . . .
H39A H 0.083206 0.276062 0.066799 0.078 Uiso 1 1 calc R U . . .
H39B H -0.045974 0.303507 0.089970 0.078 Uiso 1 1 calc R U . . .
H39C H 0.041392 0.246120 0.181989 0.078 Uiso 1 1 calc R U . . .
C40 C 0.0663(8) 0.3585(4) 0.3250(9) 0.054(2) Uani 1 1 d . . . . .
H40A H 0.068367 0.321356 0.383151 0.081 Uiso 1 1 calc R U . . .
H40B H -0.026532 0.371140 0.276025 0.081 Uiso 1 1 calc R U . . .
H40C H 0.114386 0.395958 0.377786 0.081 Uiso 1 1 calc R U . . .
C51 C -0.0048(10) 0.6065(5) 0.1178(9) 0.064(3) Uani 1 1 d . . . . .
H51 H -0.057611 0.591161 0.026510 0.077 Uiso 1 1 calc R U . . .
Cl1 Cl 0.0445(4) 0.5379(2) 0.2147(3) 0.1094(12) Uani 1 1 d . . . . .
Cl2 Cl 0.1287(3) 0.6502(2) 0.1107(4) 0.1224(13) Uani 1 1 d . . . . .
Cl3 Cl -0.1070(4) 0.6572(2) 0.1665(4) 0.1256(14) Uani 1 1 d . . . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C2 2.035(6) . ?
Fe1 C22 2.038(6) . ?
Fe1 C23 2.041(6) . ?
Fe1 C24 2.042(6) . ?
Fe1 C3 2.043(6) . ?
Fe1 C4 2.046(6) . ?
Fe1 C21 2.062(5) . ?
Fe1 C5 2.071(5) . ?
Fe1 C1 2.096(6) . ?
Fe1 C25 2.107(6) . ?
C1 C2 1.433(8) . ?
C1 C5 1.454(9) . ?
C1 Si1 1.885(7) . ?
C2 C3 1.413(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.434(9) . ?
C3 C14 1.469(9) . ?
C4 C5 1.429(9) . ?
C4 H4 0.9500 . ?
C5 S1 1.780(5) . ?
Si1 C8 1.861(7) . ?
Si1 C6 1.862(7) . ?
Si1 C7 1.867(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O9 S1 1.478(5) . ?
S1 C10 1.863(6) . ?
C10 C13 1.495(11) . ?
C10 C11 1.516(10) . ?
C10 C12 1.527(9) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 O15 1.197(7) . ?
C14 O16 1.340(8) . ?
O16 C17 1.447(8) . ?
C17 C18 1.504(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.521(12) . ?
C18 C20 1.551(11) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.417(9) . ?
C21 C25 1.446(8) . ?
C21 S2 1.771(6) . ?
C22 C23 1.433(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.423(9) . ?
C23 C34 1.477(8) . ?
C24 C25 1.452(8) . ?
C24 H24 0.9500 . ?
C25 Si2 1.888(7) . ?
Si2 C26 1.863(7) . ?
Si2 C27 1.876(8) . ?
Si2 C28 1.883(7) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O29 S2 1.497(5) . ?
S2 C30 1.865(6) . ?
C30 C32 1.480(13) . ?
C30 C33 1.520(9) . ?
C30 C31 1.538(10) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 O35 1.203(8) . ?
C34 O36 1.334(7) . ?
O36 C37 1.450(7) . ?
C37 C38 1.476(10) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C40 1.506(11) . ?
C38 C39 1.548(10) . ?
C38 H38 1.0000 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C51 Cl1 1.712(10) . ?
C51 Cl2 1.713(10) . ?
C51 Cl3 1.725(11) . ?
C51 H51 1.0000 . ?

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
C2 Fe1 C22 128.6(2) . . ?
C2 Fe1 C23 106.5(2) . . ?
C22 Fe1 C23 41.1(2) . . ?
C2 Fe1 C24 115.6(2) . . ?
C22 Fe1 C24 68.9(2) . . ?
C23 Fe1 C24 40.8(2) . . ?
C2 Fe1 C3 40.6(2) . . ?
C22 Fe1 C3 165.5(3) . . ?
C23 Fe1 C3 126.1(2) . . ?
C24 Fe1 C3 105.5(2) . . ?
C2 Fe1 C4 68.5(2) . . ?
C22 Fe1 C4 152.7(2) . . ?
C23 Fe1 C4 165.0(2) . . ?
C24 Fe1 C4 127.2(2) . . ?
C3 Fe1 C4 41.1(2) . . ?
C2 Fe1 C21 168.0(3) . . ?
C22 Fe1 C21 40.4(3) . . ?
C23 Fe1 C21 68.0(2) . . ?
C24 Fe1 C21 67.9(2) . . ?
C3 Fe1 C21 151.3(3) . . ?
C4 Fe1 C21 119.5(2) . . ?
C2 Fe1 C5 67.5(2) . . ?
C22 Fe1 C5 120.0(2) . . ?
C23 Fe1 C5 152.2(3) . . ?
C24 Fe1 C5 167.0(3) . . ?
C3 Fe1 C5 68.1(2) . . ?
C4 Fe1 C5 40.6(3) . . ?
C21 Fe1 C5 111.9(2) . . ?
C2 Fe1 C1 40.6(2) . . ?
C22 Fe1 C1 108.5(3) . . ?
C23 Fe1 C1 116.7(2) . . ?
C24 Fe1 C1 149.1(2) . . ?
C3 Fe1 C1 69.1(2) . . ?
C4 Fe1 C1 69.5(2) . . ?
C21 Fe1 C1 131.1(2) . . ?
C5 Fe1 C1 40.9(2) . . ?
C2 Fe1 C25 149.1(2) . . ?
C22 Fe1 C25 69.2(2) . . ?
C23 Fe1 C25 69.0(2) . . ?
C24 Fe1 C25 40.9(2) . . ?
C3 Fe1 C25 115.9(2) . . ?
C4 Fe1 C25 107.4(3) . . ?
C21 Fe1 C25 40.6(2) . . ?
C5 Fe1 C25 130.4(2) . . ?
C1 Fe1 C25 169.2(2) . . ?
C2 C1 C5 104.4(5) . . ?
C2 C1 Si1 121.3(5) . . ?
C5 C1 Si1 134.2(5) . . ?
C2 C1 Fe1 67.4(3) . . ?
C5 C1 Fe1 68.7(3) . . ?
Si1 C1 Fe1 130.4(3) . . ?
C3 C2 C1 111.0(6) . . ?
C3 C2 Fe1 70.0(4) . . ?
C1 C2 Fe1 72.0(3) . . ?
C3 C2 H2 124.5 . . ?
C1 C2 H2 124.5 . . ?
Fe1 C2 H2 125.1 . . ?
C2 C3 C4 107.6(6) . . ?
C2 C3 C14 125.2(6) . . ?
C4 C3 C14 127.2(6) . . ?
C2 C3 Fe1 69.4(4) . . ?
C4 C3 Fe1 69.6(3) . . ?
C14 C3 Fe1 125.1(4) . . ?
C5 C4 C3 107.1(5) . . ?
C5 C4 Fe1 70.6(3) . . ?
C3 C4 Fe1 69.3(3) . . ?
C5 C4 H4 126.5 . . ?
C3 C4 H4 126.5 . . ?
Fe1 C4 H4 125.1 . . ?
C4 C5 C1 109.9(5) . . ?
C4 C5 S1 123.1(5) . . ?
C1 C5 S1 126.7(5) . . ?
C4 C5 Fe1 68.7(3) . . ?
C1 C5 Fe1 70.5(3) . . ?
S1 C5 Fe1 123.3(3) . . ?
C8 Si1 C6 107.7(3) . . ?
C8 Si1 C7 111.3(4) . . ?
C6 Si1 C7 106.7(3) . . ?
C8 Si1 C1 110.1(3) . . ?
C6 Si1 C1 105.3(3) . . ?
C7 Si1 C1 115.3(3) . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O9 S1 C5 105.9(3) . . ?
O9 S1 C10 106.9(3) . . ?
C5 S1 C10 100.9(3) . . ?
C13 C10 C11 113.1(7) . . ?
C13 C10 C12 110.5(7) . . ?
C11 C10 C12 110.8(6) . . ?
C13 C10 S1 108.1(5) . . ?
C11 C10 S1 110.4(5) . . ?
C12 C10 S1 103.3(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O15 C14 O16 124.6(6) . . ?
O15 C14 C3 124.1(6) . . ?
O16 C14 C3 111.3(5) . . ?
C14 O16 C17 115.7(5) . . ?
O16 C17 C18 108.0(6) . . ?
O16 C17 H17A 110.1 . . ?
C18 C17 H17A 110.1 . . ?
O16 C17 H17B 110.1 . . ?
C18 C17 H17B 110.1 . . ?
H17A C17 H17B 108.4 . . ?
C17 C18 C19 110.2(7) . . ?
C17 C18 C20 108.0(7) . . ?
C19 C18 C20 112.3(7) . . ?
C17 C18 H18 108.8 . . ?
C19 C18 H18 108.8 . . ?
C20 C18 H18 108.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C25 110.5(5) . . ?
C22 C21 S2 124.5(5) . . ?
C25 C21 S2 125.0(5) . . ?
C22 C21 Fe1 68.9(3) . . ?
C25 C21 Fe1 71.4(3) . . ?
S2 C21 Fe1 125.5(3) . . ?
C21 C22 C23 107.3(5) . . ?
C21 C22 Fe1 70.7(3) . . ?
C23 C22 Fe1 69.6(3) . . ?
C21 C22 H22 126.3 . . ?
C23 C22 H22 126.3 . . ?
Fe1 C22 H22 125.0 . . ?
C24 C23 C22 107.9(6) . . ?
C24 C23 C34 127.8(6) . . ?
C22 C23 C34 124.3(6) . . ?
C24 C23 Fe1 69.6(3) . . ?
C22 C23 Fe1 69.3(3) . . ?
C34 C23 Fe1 125.4(4) . . ?
C23 C24 C25 109.7(6) . . ?
C23 C24 Fe1 69.6(4) . . ?
C25 C24 Fe1 71.9(3) . . ?
C23 C24 H24 125.1 . . ?
C25 C24 H24 125.1 . . ?
Fe1 C24 H24 124.9 . . ?
C21 C25 C24 104.5(5) . . ?
C21 C25 Si2 134.3(5) . . ?
C24 C25 Si2 121.1(5) . . ?
C21 C25 Fe1 68.0(3) . . ?
C24 C25 Fe1 67.1(3) . . ?
Si2 C25 Fe1 128.9(3) . . ?
C26 Si2 C27 106.8(4) . . ?
C26 Si2 C28 110.0(3) . . ?
C27 Si2 C28 108.3(4) . . ?
C26 Si2 C25 111.7(3) . . ?
C27 Si2 C25 104.2(3) . . ?
C28 Si2 C25 115.3(3) . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O29 S2 C21 104.5(3) . . ?
O29 S2 C30 107.7(3) . . ?
C21 S2 C30 100.4(3) . . ?
C32 C30 C33 112.3(7) . . ?
C32 C30 C31 111.0(7) . . ?
C33 C30 C31 110.6(7) . . ?
C32 C30 S2 108.1(5) . . ?
C33 C30 S2 112.0(5) . . ?
C31 C30 S2 102.4(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O35 C34 O36 124.4(6) . . ?
O35 C34 C23 123.5(6) . . ?
O36 C34 C23 112.1(5) . . ?
C34 O36 C37 115.4(5) . . ?
O36 C37 C38 109.3(5) . . ?
O36 C37 H37A 109.8 . . ?
C38 C37 H37A 109.8 . . ?
O36 C37 H37B 109.8 . . ?
C38 C37 H37B 109.8 . . ?
H37A C37 H37B 108.3 . . ?
C37 C38 C40 111.7(6) . . ?
C37 C38 C39 108.2(6) . . ?
C40 C38 C39 109.5(6) . . ?
C37 C38 H38 109.1 . . ?
C40 C38 H38 109.1 . . ?
C39 C38 H38 109.1 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
Cl1 C51 Cl2 111.8(6) . . ?
Cl1 C51 Cl3 112.6(6) . . ?
Cl2 C51 Cl3 110.1(6) . . ?
Cl1 C51 H51 107.3 . . ?
Cl2 C51 H51 107.3 . . ?
Cl3 C51 H51 107.3 . . ?

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
C5 C1 C2 C3 -0.2(7) . . . . ?
Si1 C1 C2 C3 176.0(4) . . . . ?
Fe1 C1 C2 C3 -59.4(5) . . . . ?
C5 C1 C2 Fe1 59.1(4) . . . . ?
Si1 C1 C2 Fe1 -124.6(4) . . . . ?
C1 C2 C3 C4 1.2(7) . . . . ?
Fe1 C2 C3 C4 -59.4(4) . . . . ?
C1 C2 C3 C14 179.7(5) . . . . ?
Fe1 C2 C3 C14 119.1(6) . . . . ?
C1 C2 C3 Fe1 60.5(4) . . . . ?
C2 C3 C4 C5 -1.7(6) . . . . ?
C14 C3 C4 C5 179.9(5) . . . . ?
Fe1 C3 C4 C5 -60.9(4) . . . . ?
C2 C3 C4 Fe1 59.2(4) . . . . ?
C14 C3 C4 Fe1 -119.2(6) . . . . ?
C3 C4 C5 C1 1.6(6) . . . . ?
Fe1 C4 C5 C1 -58.5(3) . . . . ?
C3 C4 C5 S1 176.8(4) . . . . ?
Fe1 C4 C5 S1 116.7(4) . . . . ?
C3 C4 C5 Fe1 60.1(4) . . . . ?
C2 C1 C5 C4 -0.8(5) . . . . ?
Si1 C1 C5 C4 -176.3(5) . . . . ?
Fe1 C1 C5 C4 57.5(3) . . . . ?
C2 C1 C5 S1 -175.9(4) . . . . ?
Si1 C1 C5 S1 8.6(8) . . . . ?
Fe1 C1 C5 S1 -117.6(4) . . . . ?
C2 C1 C5 Fe1 -58.3(4) . . . . ?
Si1 C1 C5 Fe1 126.2(5) . . . . ?
C2 C1 Si1 C8 -112.2(5) . . . . ?
C5 C1 Si1 C8 62.7(6) . . . . ?
Fe1 C1 Si1 C8 162.0(4) . . . . ?
C2 C1 Si1 C6 3.7(5) . . . . ?
C5 C1 Si1 C6 178.6(6) . . . . ?
Fe1 C1 Si1 C6 -82.1(5) . . . . ?
C2 C1 Si1 C7 120.9(5) . . . . ?
C5 C1 Si1 C7 -64.2(6) . . . . ?
Fe1 C1 Si1 C7 35.1(5) . . . . ?
C4 C5 S1 O9 -176.0(4) . . . . ?
C1 C5 S1 O9 -1.6(5) . . . . ?
Fe1 C5 S1 O9 -91.1(4) . . . . ?
C4 C5 S1 C10 72.7(5) . . . . ?
C1 C5 S1 C10 -112.9(5) . . . . ?
Fe1 C5 S1 C10 157.6(4) . . . . ?
O9 S1 C10 C13 -178.7(6) . . . . ?
C5 S1 C10 C13 -68.2(6) . . . . ?
O9 S1 C10 C11 -54.5(6) . . . . ?
C5 S1 C10 C11 56.0(6) . . . . ?
O9 S1 C10 C12 64.1(6) . . . . ?
C5 S1 C10 C12 174.6(5) . . . . ?
C2 C3 C14 O15 -8.1(10) . . . . ?
C4 C3 C14 O15 170.1(6) . . . . ?
Fe1 C3 C14 O15 80.1(8) . . . . ?
C2 C3 C14 O16 169.9(6) . . . . ?
C4 C3 C14 O16 -11.9(8) . . . . ?
Fe1 C3 C14 O16 -101.8(6) . . . . ?
O15 C14 O16 C17 0.7(8) . . . . ?
C3 C14 O16 C17 -177.4(5) . . . . ?
C14 O16 C17 C18 -177.2(6) . . . . ?
O16 C17 C18 C19 -63.3(8) . . . . ?
O16 C17 C18 C20 173.8(6) . . . . ?
C25 C21 C22 C23 0.9(6) . . . . ?
S2 C21 C22 C23 179.6(4) . . . . ?
Fe1 C21 C22 C23 60.2(4) . . . . ?
C25 C21 C22 Fe1 -59.3(4) . . . . ?
S2 C21 C22 Fe1 119.4(4) . . . . ?
C21 C22 C23 C24 -1.8(6) . . . . ?
Fe1 C22 C23 C24 59.2(4) . . . . ?
C21 C22 C23 C34 179.5(5) . . . . ?
Fe1 C22 C23 C34 -119.5(5) . . . . ?
C21 C22 C23 Fe1 -61.0(4) . . . . ?
C22 C23 C24 C25 2.0(7) . . . . ?
C34 C23 C24 C25 -179.4(5) . . . . ?
Fe1 C23 C24 C25 61.0(4) . . . . ?
C22 C23 C24 Fe1 -58.9(4) . . . . ?
C34 C23 C24 Fe1 119.7(6) . . . . ?
C22 C21 C25 C24 0.3(6) . . . . ?
S2 C21 C25 C24 -178.4(4) . . . . ?
Fe1 C21 C25 C24 -57.5(4) . . . . ?
C22 C21 C25 Si2 -178.6(5) . . . . ?
S2 C21 C25 Si2 2.7(8) . . . . ?
Fe1 C21 C25 Si2 123.5(5) . . . . ?
C22 C21 C25 Fe1 57.8(4) . . . . ?
S2 C21 C25 Fe1 -120.8(4) . . . . ?
C23 C24 C25 C21 -1.4(6) . . . . ?
Fe1 C24 C25 C21 58.1(4) . . . . ?
C23 C24 C25 Si2 177.7(4) . . . . ?
Fe1 C24 C25 Si2 -122.8(4) . . . . ?
C23 C24 C25 Fe1 -59.5(4) . . . . ?
C21 C25 Si2 C26 63.2(6) . . . . ?
C24 C25 Si2 C26 -115.6(5) . . . . ?
Fe1 C25 Si2 C26 159.9(4) . . . . ?
C21 C25 Si2 C27 178.2(6) . . . . ?
C24 C25 Si2 C27 -0.6(5) . . . . ?
Fe1 C25 Si2 C27 -85.2(4) . . . . ?
C21 C25 Si2 C28 -63.3(7) . . . . ?
C24 C25 Si2 C28 117.9(5) . . . . ?
Fe1 C25 Si2 C28 33.4(5) . . . . ?
C22 C21 S2 O29 -175.4(5) . . . . ?
C25 C21 S2 O29 3.0(5) . . . . ?
Fe1 C21 S2 O29 -88.2(5) . . . . ?
C22 C21 S2 C30 73.0(5) . . . . ?
C25 C21 S2 C30 -108.5(5) . . . . ?
Fe1 C21 S2 C30 160.3(5) . . . . ?
O29 S2 C30 C32 173.0(5) . . . . ?
C21 S2 C30 C32 -78.0(6) . . . . ?
O29 S2 C30 C33 -62.8(6) . . . . ?
C21 S2 C30 C33 46.2(7) . . . . ?
O29 S2 C30 C31 55.8(6) . . . . ?
C21 S2 C30 C31 164.8(6) . . . . ?
C24 C23 C34 O35 167.0(6) . . . . ?
C22 C23 C34 O35 -14.5(9) . . . . ?
Fe1 C23 C34 O35 -102.3(7) . . . . ?
C24 C23 C34 O36 -11.2(8) . . . . ?
C22 C23 C34 O36 167.2(5) . . . . ?
Fe1 C23 C34 O36 79.5(6) . . . . ?
O35 C34 O36 C37 -1.0(8) . . . . ?
C23 C34 O36 C37 177.3(5) . . . . ?
C34 O36 C37 C38 167.7(5) . . . . ?
O36 C37 C38 C40 -63.4(8) . . . . ?
O36 C37 C38 C39 176.1(5) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_MW578
_database_code_depnum_ccdc_archive 'CCDC 2204518'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-30 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 22 fevrier 2022                                          #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C27 H28 Fe O2 S'
_chemical_formula_sum            'C27 H28 Fe O2 S'
_chemical_formula_weight         472.40
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      tetragonal
_space_group_name_H-M_alt        'P 43'
_space_group_name_Hall           'P 4cw'
_space_group_IT_number           78
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'

_cell_length_a                   9.1285(3)
_cell_length_b                   9.1285
_cell_length_c                   27.3023(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2275.09(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7907
_cell_measurement_theta_min      2.3525
_cell_measurement_theta_max      27.3318
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0036602
_diffrn_orient_matrix_UB_21      -0.0451112
_diffrn_orient_matrix_UB_31      0.0997604
_diffrn_orient_matrix_UB_12      -0.0824446
_diffrn_orient_matrix_UB_22      0.0645436
_diffrn_orient_matrix_UB_32      0.0322112
_diffrn_orient_matrix_UB_13      -0.0240871
_diffrn_orient_matrix_UB_23      -0.0254625
_diffrn_orient_matrix_UB_33      -0.0106303


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.580
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.460
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             992
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_T_max  0.700

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS 2014.5.0.0/23-May-2014 && APEX2_2014.11-0   #
# Number of scans            :        5                                        #
# Total number of frames     :      467                                        #
# Total length of scans      :   467.00 (deg.)                                 #
# Rotation speed             :     5.00 sec./deg.                              #
# Total exposition time      :         38.9 min.                               #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Omega    5.0  1.00    35.0    93   93.0  344.0  343.5  122.7  -28.9 150.0 #
#  2 Omega    5.0  1.00    35.0    93   93.0  344.0  341.2  331.9  -23.7 150.0 #
#  3 Omega    5.0  1.00    35.0    93   93.0  344.0  343.5  122.7  -28.9 150.0 #
#  4 Omega    5.0  1.00    35.0    93   93.0  344.0  341.2  331.9  -23.7 150.0 #
#  5 Omega    5.0  1.00    35.0    95   95.0  344.0  252.4  125.9   27.2 150.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_detector_area_resol_mean 8.33
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0396
_diffrn_reflns_av_r_equivalents  0.0394
_diffrn_reflns_number            22654
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.684
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             5190
_reflns_number_gt                4871
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0272P)²+0.9403P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         5190
_refine_ls_number_parameters     286
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0674
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
Flack x determined using 2135 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(8)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.18265(5) 0.62465(5) 0.49051(2) 0.01910(11) Uani 1 1 d . . . . .
C1 C 0.2147(4) 0.4959(4) 0.55090(16) 0.0361(10) Uani 1 1 d . . . . .
H1 H 0.294600 0.502691 0.573074 0.043 Uiso 1 1 calc R U . . .
C2 C 0.0793(4) 0.5699(4) 0.55505(14) 0.0306(8) Uani 1 1 d . . . . .
H2 H 0.052172 0.635395 0.580522 0.037 Uiso 1 1 calc R U . . .
C3 C -0.0093(4) 0.5292(4) 0.51441(15) 0.0320(8) Uani 1 1 d . . . . .
H3 H -0.105994 0.562657 0.508003 0.038 Uiso 1 1 calc R U . . .
C4 C 0.0712(4) 0.4306(4) 0.48537(17) 0.0365(9) Uani 1 1 d . . . . .
H4 H 0.038371 0.385859 0.455937 0.044 Uiso 1 1 calc R U . . .
C5 C 0.2099(4) 0.4096(4) 0.50761(17) 0.0397(11) Uani 1 1 d . . . . .
H5 H 0.286249 0.348478 0.495687 0.048 Uiso 1 1 calc R U . . .
C6 C 0.2432(4) 0.6801(4) 0.42113(12) 0.0221(7) Uani 1 1 d . . . . .
H6 H 0.239183 0.618185 0.393192 0.027 Uiso 1 1 calc R U . . .
C7 C 0.1311(4) 0.7747(4) 0.43752(13) 0.0243(7) Uani 1 1 d . . . . .
H7 H 0.038636 0.788108 0.422195 0.029 Uiso 1 1 calc R U . . .
C8 C 0.1796(3) 0.8468(3) 0.48083(12) 0.0213(7) Uani 1 1 d . . . . .
H8 H 0.124633 0.916493 0.498998 0.026 Uiso 1 1 calc R U . . .
C9 C 0.3244(3) 0.7978(3) 0.49269(13) 0.0166(6) Uani 1 1 d . . . . .
C10 C 0.3642(3) 0.6945(3) 0.45434(11) 0.0163(6) Uani 1 1 d . . . . .
S1 S 0.51481(9) 0.57345(8) 0.44591(3) 0.01966(17) Uani 1 1 d . . . . .
O11 O 0.6067(2) 0.5738(3) 0.49200(10) 0.0297(5) Uani 1 1 d . . . . .
C12 C 0.6302(4) 0.6607(4) 0.39852(12) 0.0217(7) Uani 1 1 d . . . . .
C13 C 0.7512(5) 0.5472(5) 0.39025(16) 0.0404(10) Uani 1 1 d . . . . .
H13A H 0.815514 0.580186 0.363709 0.061 Uiso 1 1 calc R U . . .
H13B H 0.707038 0.453001 0.381374 0.061 Uiso 1 1 calc R U . . .
H13C H 0.808487 0.535739 0.420361 0.061 Uiso 1 1 calc R U . . .
C14 C 0.6937(5) 0.8043(4) 0.41581(16) 0.0402(10) Uani 1 1 d . . . . .
H14A H 0.766601 0.838759 0.392128 0.060 Uiso 1 1 calc R U . . .
H14B H 0.740415 0.790402 0.447785 0.060 Uiso 1 1 calc R U . . .
H14C H 0.615161 0.877010 0.418744 0.060 Uiso 1 1 calc R U . . .
C15 C 0.5397(5) 0.6772(5) 0.35223(14) 0.0434(11) Uani 1 1 d . . . . .
H15A H 0.466438 0.754426 0.356956 0.065 Uiso 1 1 calc R U . . .
H15B H 0.490192 0.584472 0.344968 0.065 Uiso 1 1 calc R U . . .
H15C H 0.603996 0.703488 0.324856 0.065 Uiso 1 1 calc R U . . .
C16 C 0.4159(3) 0.8547(3) 0.53595(11) 0.0176(6) Uani 1 1 d . . . . .
O17 O 0.4902(3) 0.7394(3) 0.56017(9) 0.0220(5) Uani 1 1 d D . . . .
H17 H 0.532(4) 0.697(4) 0.5382(12) 0.026 Uiso 1 1 d D U . . .
C18 C 0.3125(3) 0.9221(4) 0.57451(12) 0.0195(7) Uani 1 1 d . . . . .
C19 C 0.2640(4) 0.8369(4) 0.61347(12) 0.0246(7) Uani 1 1 d . . . . .
H19 H 0.299929 0.739900 0.617372 0.030 Uiso 1 1 calc R U . . .
C20 C 0.1627(4) 0.8930(4) 0.64690(13) 0.0281(8) Uani 1 1 d . . . . .
H20 H 0.129364 0.833353 0.673151 0.034 Uiso 1 1 calc R U . . .
C21 C 0.1105(4) 1.0342(4) 0.64218(13) 0.0276(8) Uani 1 1 d . . . . .
H21 H 0.041231 1.071715 0.664910 0.033 Uiso 1 1 calc R U . . .
C22 C 0.1601(4) 1.1203(4) 0.60407(14) 0.0288(8) Uani 1 1 d . . . . .
H22 H 0.125554 1.217950 0.600808 0.035 Uiso 1 1 calc R U . . .
C23 C 0.2598(4) 1.0653(4) 0.57053(14) 0.0256(8) Uani 1 1 d . . . . .
H23 H 0.292907 1.125767 0.544470 0.031 Uiso 1 1 calc R U . . .
C24 C 0.5263(4) 0.9703(4) 0.51786(13) 0.0229(7) Uani 1 1 d . . . . .
C25 C 0.4920(4) 1.0683(4) 0.48041(14) 0.0308(9) Uani 1 1 d . . . . .
H25 H 0.399924 1.061136 0.464388 0.037 Uiso 1 1 calc R U . . .
C26 C 0.5903(5) 1.1761(4) 0.46617(18) 0.0451(12) Uani 1 1 d . . . . .
H26 H 0.565060 1.242459 0.440740 0.054 Uiso 1 1 calc R U . . .
C27 C 0.7252(5) 1.1868(5) 0.4890(2) 0.0539(14) Uani 1 1 d . . . . .
H27 H 0.792160 1.261596 0.479844 0.065 Uiso 1 1 calc R U . . .
C28 C 0.7615(5) 1.0888(6) 0.52503(18) 0.0508(13) Uani 1 1 d . . . . .
H28 H 0.855168 1.094436 0.540083 0.061 Uiso 1 1 calc R U . . .
C29 C 0.6631(4) 0.9808(5) 0.53992(14) 0.0351(9) Uani 1 1 d . . . . .
H29 H 0.689635 0.914340 0.565178 0.042 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C10 2.031(3) . ?
Fe1 C5 2.033(4) . ?
Fe1 C6 2.037(3) . ?
Fe1 C9 2.044(3) . ?
Fe1 C8 2.046(3) . ?
Fe1 C1 2.046(4) . ?
Fe1 C7 2.047(3) . ?
Fe1 C4 2.047(3) . ?
Fe1 C2 2.060(4) . ?
Fe1 C3 2.063(4) . ?
C1 C2 1.413(6) . ?
C1 C5 1.421(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.423(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.407(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.417(6) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.412(5) . ?
C6 C10 1.435(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.424(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.432(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.455(4) . ?
C9 C16 1.537(4) . ?
C10 S1 1.779(3) . ?
S1 O11 1.512(3) . ?
S1 C12 1.849(3) . ?
C12 C14 1.509(5) . ?
C12 C15 1.518(5) . ?
C12 C13 1.531(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 O17 1.416(4) . ?
C16 C24 1.540(4) . ?
C16 C18 1.542(4) . ?
O17 H17 0.81(2) . ?
C18 C19 1.390(5) . ?
C18 C23 1.397(5) . ?
C19 C20 1.397(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(5) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.390(5) . ?
C24 C25 1.394(5) . ?
C25 C26 1.387(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.370(8) . ?
C27 H27 0.9500 . ?
C28 C29 1.394(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?

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
C10 Fe1 C5 108.34(14) . . ?
C10 Fe1 C6 41.31(12) . . ?
C5 Fe1 C6 114.85(16) . . ?
C10 Fe1 C9 41.85(12) . . ?
C5 Fe1 C9 131.51(15) . . ?
C6 Fe1 C9 70.32(14) . . ?
C10 Fe1 C8 68.72(12) . . ?
C5 Fe1 C8 171.38(16) . . ?
C6 Fe1 C8 68.72(14) . . ?
C9 Fe1 C8 41.00(12) . . ?
C10 Fe1 C1 117.09(14) . . ?
C5 Fe1 C1 40.78(18) . . ?
C6 Fe1 C1 148.59(16) . . ?
C9 Fe1 C1 109.29(15) . . ?
C8 Fe1 C1 132.51(16) . . ?
C10 Fe1 C7 68.53(13) . . ?
C5 Fe1 C7 146.77(17) . . ?
C6 Fe1 C7 40.44(13) . . ?
C9 Fe1 C7 69.42(13) . . ?
C8 Fe1 C7 40.72(13) . . ?
C1 Fe1 C7 170.69(17) . . ?
C10 Fe1 C4 130.03(14) . . ?
C5 Fe1 C4 40.63(17) . . ?
C6 Fe1 C4 106.61(16) . . ?
C9 Fe1 C4 170.30(14) . . ?
C8 Fe1 C4 147.39(15) . . ?
C1 Fe1 C4 68.24(17) . . ?
C7 Fe1 C4 114.61(16) . . ?
C10 Fe1 C2 149.93(14) . . ?
C5 Fe1 C2 68.01(17) . . ?
C6 Fe1 C2 168.45(15) . . ?
C9 Fe1 C2 116.92(14) . . ?
C8 Fe1 C2 110.18(15) . . ?
C1 Fe1 C2 40.26(16) . . ?
C7 Fe1 C2 131.41(15) . . ?
C4 Fe1 C2 67.75(16) . . ?
C10 Fe1 C3 168.26(14) . . ?
C5 Fe1 C3 67.88(16) . . ?
C6 Fe1 C3 129.00(15) . . ?
C9 Fe1 C3 148.80(14) . . ?
C8 Fe1 C3 116.64(14) . . ?
C1 Fe1 C3 67.91(16) . . ?
C7 Fe1 C3 108.12(15) . . ?
C4 Fe1 C3 40.03(15) . . ?
C2 Fe1 C3 40.36(15) . . ?
C2 C1 C5 107.8(4) . . ?
C2 C1 Fe1 70.4(2) . . ?
C5 C1 Fe1 69.1(2) . . ?
C2 C1 H1 126.1 . . ?
C5 C1 H1 126.1 . . ?
Fe1 C1 H1 125.9 . . ?
C1 C2 C3 108.1(4) . . ?
C1 C2 Fe1 69.3(2) . . ?
C3 C2 Fe1 69.9(2) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
Fe1 C2 H2 126.4 . . ?
C4 C3 C2 108.0(4) . . ?
C4 C3 Fe1 69.4(2) . . ?
C2 C3 Fe1 69.7(2) . . ?
C4 C3 H3 126.0 . . ?
C2 C3 H3 126.0 . . ?
Fe1 C3 H3 126.5 . . ?
C3 C4 C5 108.2(4) . . ?
C3 C4 Fe1 70.6(2) . . ?
C5 C4 Fe1 69.2(2) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Fe1 C4 H4 125.9 . . ?
C4 C5 C1 108.0(4) . . ?
C4 C5 Fe1 70.2(2) . . ?
C1 C5 Fe1 70.1(2) . . ?
C4 C5 H5 126.0 . . ?
C1 C5 H5 126.0 . . ?
Fe1 C5 H5 125.3 . . ?
C7 C6 C10 107.5(3) . . ?
C7 C6 Fe1 70.2(2) . . ?
C10 C6 Fe1 69.13(18) . . ?
C7 C6 H6 126.2 . . ?
C10 C6 H6 126.2 . . ?
Fe1 C6 H6 126.0 . . ?
C6 C7 C8 108.7(3) . . ?
C6 C7 Fe1 69.39(19) . . ?
C8 C7 Fe1 69.57(19) . . ?
C6 C7 H7 125.6 . . ?
C8 C7 H7 125.6 . . ?
Fe1 C7 H7 127.0 . . ?
C7 C8 C9 109.3(3) . . ?
C7 C8 Fe1 69.71(18) . . ?
C9 C8 Fe1 69.43(17) . . ?
C7 C8 H8 125.4 . . ?
C9 C8 H8 125.4 . . ?
Fe1 C8 H8 127.1 . . ?
C8 C9 C10 105.7(3) . . ?
C8 C9 C16 124.7(3) . . ?
C10 C9 C16 129.5(3) . . ?
C8 C9 Fe1 69.57(17) . . ?
C10 C9 Fe1 68.63(16) . . ?
C16 C9 Fe1 128.9(2) . . ?
C6 C10 C9 108.8(3) . . ?
C6 C10 S1 117.2(2) . . ?
C9 C10 S1 133.5(2) . . ?
C6 C10 Fe1 69.56(18) . . ?
C9 C10 Fe1 69.52(16) . . ?
S1 C10 Fe1 119.90(16) . . ?
O11 S1 C10 108.66(14) . . ?
O11 S1 C12 105.40(15) . . ?
C10 S1 C12 105.28(15) . . ?
C14 C12 C15 112.5(3) . . ?
C14 C12 C13 110.9(3) . . ?
C15 C12 C13 109.7(3) . . ?
C14 C12 S1 112.0(3) . . ?
C15 C12 S1 108.4(2) . . ?
C13 C12 S1 102.9(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O17 C16 C9 111.6(2) . . ?
O17 C16 C24 110.2(3) . . ?
C9 C16 C24 109.9(3) . . ?
O17 C16 C18 105.7(2) . . ?
C9 C16 C18 109.1(2) . . ?
C24 C16 C18 110.3(3) . . ?
C16 O17 H17 104(3) . . ?
C19 C18 C23 118.3(3) . . ?
C19 C18 C16 119.6(3) . . ?
C23 C18 C16 122.0(3) . . ?
C18 C19 C20 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C21 C20 C19 120.7(3) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C22 C21 C20 119.3(3) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C23 120.5(3) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C18 120.9(3) . . ?
C22 C23 H23 119.5 . . ?
C18 C23 H23 119.5 . . ?
C29 C24 C25 118.3(3) . . ?
C29 C24 C16 119.8(3) . . ?
C25 C24 C16 121.9(3) . . ?
C26 C25 C24 121.1(4) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C27 C26 C25 119.9(5) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 119.5(4) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C29 121.0(4) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C24 C29 C28 120.1(4) . . ?
C24 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?

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
C5 C1 C2 C3 0.1(4) . . . . ?
Fe1 C1 C2 C3 59.4(3) . . . . ?
C5 C1 C2 Fe1 -59.3(2) . . . . ?
C1 C2 C3 C4 0.0(4) . . . . ?
Fe1 C2 C3 C4 59.0(3) . . . . ?
C1 C2 C3 Fe1 -59.0(2) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
Fe1 C3 C4 C5 59.1(2) . . . . ?
C2 C3 C4 Fe1 -59.2(3) . . . . ?
C3 C4 C5 C1 0.1(4) . . . . ?
Fe1 C4 C5 C1 60.2(2) . . . . ?
C3 C4 C5 Fe1 -60.0(3) . . . . ?
C2 C1 C5 C4 -0.1(4) . . . . ?
Fe1 C1 C5 C4 -60.2(3) . . . . ?
C2 C1 C5 Fe1 60.1(2) . . . . ?
C10 C6 C7 C8 -0.7(4) . . . . ?
Fe1 C6 C7 C8 58.6(2) . . . . ?
C10 C6 C7 Fe1 -59.3(2) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
Fe1 C7 C8 C9 58.2(2) . . . . ?
C6 C7 C8 Fe1 -58.5(2) . . . . ?
C7 C8 C9 C10 1.0(3) . . . . ?
Fe1 C8 C9 C10 59.45(19) . . . . ?
C7 C8 C9 C16 177.7(3) . . . . ?
Fe1 C8 C9 C16 -123.8(3) . . . . ?
C7 C8 C9 Fe1 -58.4(2) . . . . ?
C7 C6 C10 C9 1.3(4) . . . . ?
Fe1 C6 C10 C9 -58.6(2) . . . . ?
C7 C6 C10 S1 173.9(2) . . . . ?
Fe1 C6 C10 S1 114.0(2) . . . . ?
C7 C6 C10 Fe1 59.9(2) . . . . ?
C8 C9 C10 C6 -1.4(3) . . . . ?
C16 C9 C10 C6 -177.9(3) . . . . ?
Fe1 C9 C10 C6 58.6(2) . . . . ?
C8 C9 C10 S1 -172.4(3) . . . . ?
C16 C9 C10 S1 11.2(5) . . . . ?
Fe1 C9 C10 S1 -112.3(3) . . . . ?
C8 C9 C10 Fe1 -60.1(2) . . . . ?
C16 C9 C10 Fe1 123.4(3) . . . . ?
C6 C10 S1 O11 -163.2(2) . . . . ?
C9 C10 S1 O11 7.2(3) . . . . ?
Fe1 C10 S1 O11 -82.2(2) . . . . ?
C6 C10 S1 C12 84.3(3) . . . . ?
C9 C10 S1 C12 -105.3(3) . . . . ?
Fe1 C10 S1 C12 165.26(17) . . . . ?
O11 S1 C12 C14 -50.1(3) . . . . ?
C10 S1 C12 C14 64.7(3) . . . . ?
O11 S1 C12 C15 -174.8(3) . . . . ?
C10 S1 C12 C15 -60.0(3) . . . . ?
O11 S1 C12 C13 69.1(3) . . . . ?
C10 S1 C12 C13 -176.1(2) . . . . ?
C8 C9 C16 O17 138.3(3) . . . . ?
C10 C9 C16 O17 -45.9(4) . . . . ?
Fe1 C9 C16 O17 47.5(4) . . . . ?
C8 C9 C16 C24 -99.2(3) . . . . ?
C10 C9 C16 C24 76.7(4) . . . . ?
Fe1 C9 C16 C24 170.1(2) . . . . ?
C8 C9 C16 C18 21.8(4) . . . . ?
C10 C9 C16 C18 -162.3(3) . . . . ?
Fe1 C9 C16 C18 -68.9(3) . . . . ?
O17 C16 C18 C19 -25.6(4) . . . . ?
C9 C16 C18 C19 94.5(3) . . . . ?
C24 C16 C18 C19 -144.7(3) . . . . ?
O17 C16 C18 C23 157.3(3) . . . . ?
C9 C16 C18 C23 -82.6(4) . . . . ?
C24 C16 C18 C23 38.2(4) . . . . ?
C23 C18 C19 C20 1.4(5) . . . . ?
C16 C18 C19 C20 -175.7(3) . . . . ?
C18 C19 C20 C21 -0.8(5) . . . . ?
C19 C20 C21 C22 -0.3(5) . . . . ?
C20 C21 C22 C23 0.7(5) . . . . ?
C21 C22 C23 C18 -0.1(6) . . . . ?
C19 C18 C23 C22 -1.0(5) . . . . ?
C16 C18 C23 C22 176.1(3) . . . . ?
O17 C16 C24 C29 -22.5(4) . . . . ?
C9 C16 C24 C29 -145.9(3) . . . . ?
C18 C16 C24 C29 93.9(4) . . . . ?
O17 C16 C24 C25 159.1(3) . . . . ?
C9 C16 C24 C25 35.7(4) . . . . ?
C18 C16 C24 C25 -84.6(4) . . . . ?
C29 C24 C25 C26 -1.5(5) . . . . ?
C16 C24 C25 C26 176.9(3) . . . . ?
C24 C25 C26 C27 0.4(6) . . . . ?
C25 C26 C27 C28 1.2(6) . . . . ?
C26 C27 C28 C29 -1.8(7) . . . . ?
C25 C24 C29 C28 1.0(5) . . . . ?
C16 C24 C29 C28 -177.5(3) . . . . ?
C27 C28 C29 C24 0.7(6) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_MW514_3_200K
_database_code_depnum_ccdc_archive 'CCDC 2204519'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-30 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 09 novembre 2021                                         #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H42 Fe O2 S2 Si2'
_chemical_formula_sum            'C24 H42 Fe O2 S2 Si2'
_chemical_formula_weight         538.72
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration rm/ad/rmad/syn/unk/.

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
_space_group_IT_number           19
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.5430(3)
_cell_length_b                   12.7335(3)
_cell_length_c                   18.3899(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2937.17(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9583
_cell_measurement_theta_min      2.5342
_cell_measurement_theta_max      27.1392
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      -0.0295086
_diffrn_orient_matrix_UB_21      0.0500572
_diffrn_orient_matrix_UB_31      -0.0545868
_diffrn_orient_matrix_UB_12      -0.0674678
_diffrn_orient_matrix_UB_22      0.0038566
_diffrn_orient_matrix_UB_32      0.0400084
_diffrn_orient_matrix_UB_13      0.0192219
_diffrn_orient_matrix_UB_23      0.0422389
_diffrn_orient_matrix_UB_33      0.0283430


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1152
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.766
_exptl_absorpt_correction_T_max  0.860

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS V6.2.15/2021-03-15 && APEX4 2021.10-0       #
# Number of scans            :        2                                        #
# Total number of frames     :      151                                        #
# Total length of scans      :   151.00 (deg.)                                 #
# Rotation speed             :    10.00 sec./deg.                              #
# Total exposition time      :         25.2 min.                               #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Phi     10.0  1.00    34.0   151  151.0    1.9  272.7   72.5   23.0 200.0 #
#  2 Fast     1.0  1.00    34.0   180  180.0    0.0  360.0    0.0   54.7 200.0 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_detector                 CMOS-PHOTON70
_diffrn_detector_area_resol_mean ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_source_current           1.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0383
_diffrn_reflns_av_r_equivalents  0.0351
_diffrn_reflns_number            16742
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.534
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             6636
_reflns_number_gt                6089
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_max     0.976
_reflns_Friedel_fraction_full    0.994

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0434P)²+0.5213P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6636
_refine_ls_number_parameters     296
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 
;
Flack x determined using 2419 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(7)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Fe Fe 0.3463 0.8444 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.61390(3) 0.49378(3) 0.69248(2) 0.02783(11) Uani 1 1 d . . . . .
C1 C 0.5210(3) 0.3980(2) 0.63116(18) 0.0350(7) Uani 1 1 d . . . . .
C2 C 0.6224(3) 0.3514(2) 0.6439(2) 0.0479(9) Uani 1 1 d . . . . .
H2 H 0.672624 0.331952 0.607648 0.057 Uiso 1 1 calc R U . . .
C3 C 0.6356(3) 0.3390(2) 0.7190(2) 0.0503(10) Uani 1 1 d . . . . .
H3 H 0.695658 0.309152 0.742735 0.060 Uiso 1 1 calc R U . . .
C4 C 0.5433(3) 0.3789(3) 0.7530(2) 0.0421(8) Uani 1 1 d . . . . .
H4 H 0.531716 0.380101 0.804082 0.051 Uiso 1 1 calc R U . . .
C5 C 0.4696(2) 0.4174(2) 0.70013(16) 0.0318(6) Uani 1 1 d . . . . .
Si1 Si 0.33980(8) 0.47778(9) 0.73007(7) 0.0566(3) Uani 1 1 d . . . . .
C6 C 0.3597(6) 0.5159(7) 0.8267(4) 0.145(4) Uani 1 1 d . . . . .
H6A H 0.298904 0.558032 0.843107 0.217 Uiso 1 1 calc R U . . .
H6B H 0.425283 0.557161 0.831175 0.217 Uiso 1 1 calc R U . . .
H6C H 0.365316 0.452532 0.856698 0.217 Uiso 1 1 calc R U . . .
C7 C 0.2306(3) 0.3790(4) 0.7277(4) 0.116(3) Uani 1 1 d . . . . .
H7A H 0.256166 0.312664 0.748363 0.174 Uiso 1 1 calc R U . . .
H7B H 0.208179 0.367656 0.677287 0.174 Uiso 1 1 calc R U . . .
H7C H 0.170017 0.404662 0.756273 0.174 Uiso 1 1 calc R U . . .
C8 C 0.2976(4) 0.5966(3) 0.6803(4) 0.0813(16) Uani 1 1 d . . . . .
H8A H 0.236736 0.628764 0.705177 0.122 Uiso 1 1 calc R U . . .
H8B H 0.276892 0.577412 0.630621 0.122 Uiso 1 1 calc R U . . .
H8C H 0.356799 0.646806 0.678515 0.122 Uiso 1 1 calc R U . . .
S1 S 0.48154(11) 0.43059(9) 0.54152(5) 0.0632(3) Uani 1 1 d . . . . .
O9 O 0.3970(4) 0.5086(4) 0.5453(2) 0.134(2) Uani 1 1 d . . . . .
C10A C 0.4225(5) 0.3057(5) 0.5106(3) 0.0847(18) Uani 0.537(14) 1 d . . P A 1
C11A C 0.4887(16) 0.2180(14) 0.5198(10) 0.107(4) Uani 0.537(14) 1 d . . P A 1
H11A H 0.511490 0.213562 0.570714 0.160 Uiso 0.537(14) 1 calc R U P A 1
H11B H 0.449450 0.154171 0.506751 0.160 Uiso 0.537(14) 1 calc R U P A 1
H11C H 0.551463 0.224872 0.488445 0.160 Uiso 0.537(14) 1 calc R U P A 1
C12A C 0.3163(15) 0.2968(15) 0.5626(10) 0.098(6) Uani 0.537(14) 1 d . . P A 1
H12A H 0.271245 0.358811 0.555368 0.147 Uiso 0.537(14) 1 calc R U P A 1
H12B H 0.276161 0.233485 0.549779 0.147 Uiso 0.537(14) 1 calc R U P A 1
H12C H 0.338281 0.292922 0.613685 0.147 Uiso 0.537(14) 1 calc R U P A 1
C13A C 0.3744(7) 0.3330(6) 0.4365(3) 0.128(3) Uani 0.537(14) 1 d . . P A 1
H13A H 0.330727 0.396548 0.440941 0.193 Uiso 0.537(14) 1 calc R U P A 1
H13B H 0.431804 0.345378 0.401385 0.193 Uiso 0.537(14) 1 calc R U P A 1
H13C H 0.329792 0.274677 0.419692 0.193 Uiso 0.537(14) 1 calc R U P A 1
C10B C 0.4225(5) 0.3057(5) 0.5106(3) 0.0847(18) Uani 0.463(14) 1 d . . P A 2
C11B C 0.5301(19) 0.2392(17) 0.4869(11) 0.107(4) Uani 0.463(14) 1 d . . P A 2
H11D H 0.573536 0.281820 0.453952 0.160 Uiso 0.463(14) 1 calc R U P A 2
H11E H 0.571635 0.221986 0.530468 0.160 Uiso 0.463(14) 1 calc R U P A 2
H11F H 0.508856 0.174165 0.462329 0.160 Uiso 0.463(14) 1 calc R U P A 2
C12B C 0.3617(17) 0.2432(18) 0.5577(12) 0.098(6) Uani 0.463(14) 1 d . . P A 2
H12D H 0.401329 0.231638 0.602962 0.147 Uiso 0.463(14) 1 calc R U P A 2
H12E H 0.294288 0.278813 0.568673 0.147 Uiso 0.463(14) 1 calc R U P A 2
H12F H 0.346900 0.175478 0.534533 0.147 Uiso 0.463(14) 1 calc R U P A 2
C13B C 0.3744(7) 0.3330(6) 0.4365(3) 0.128(3) Uani 0.463(14) 1 d . . P A 2
H13D H 0.424609 0.376734 0.409097 0.193 Uiso 0.463(14) 1 calc R U P A 2
H13E H 0.360163 0.268267 0.409390 0.193 Uiso 0.463(14) 1 calc R U P A 2
H13F H 0.307551 0.371603 0.443531 0.193 Uiso 0.463(14) 1 calc R U P A 2
C21 C 0.7172(3) 0.5927(2) 0.64193(17) 0.0352(7) Uani 1 1 d . . . . .
C22 C 0.6139(3) 0.6383(2) 0.6465(2) 0.0458(8) Uani 1 1 d . . . . .
H22 H 0.570666 0.659203 0.606615 0.055 Uiso 1 1 calc R U . . .
C23 C 0.5867(3) 0.6469(2) 0.7212(2) 0.0474(9) Uani 1 1 d . . . . .
H23 H 0.522674 0.675426 0.740481 0.057 Uiso 1 1 calc R U . . .
C24 C 0.6718(3) 0.6057(2) 0.76119(19) 0.0390(7) Uani 1 1 d . . . . .
H24 H 0.673786 0.601796 0.812756 0.047 Uiso 1 1 calc R U . . .
C25 C 0.7552(2) 0.5703(2) 0.71450(16) 0.0312(6) Uani 1 1 d . . . . .
Si2 Si 0.87985(7) 0.50954(8) 0.75299(7) 0.0514(3) Uani 1 1 d . . . . .
C26 C 0.9152(4) 0.3783(4) 0.7174(5) 0.136(3) Uani 1 1 d . . . . .
H26A H 0.973523 0.348784 0.746389 0.204 Uiso 1 1 calc R U . . .
H26B H 0.937974 0.384651 0.666588 0.204 Uiso 1 1 calc R U . . .
H26C H 0.853002 0.332002 0.720301 0.204 Uiso 1 1 calc R U . . .
C27 C 0.8530(5) 0.4921(7) 0.8517(3) 0.140(4) Uani 1 1 d . . . . .
H27A H 0.792307 0.444494 0.858137 0.209 Uiso 1 1 calc R U . . .
H27B H 0.836430 0.560295 0.873562 0.209 Uiso 1 1 calc R U . . .
H27C H 0.916094 0.462158 0.875309 0.209 Uiso 1 1 calc R U . . .
C28 C 0.9948(3) 0.5996(4) 0.7441(3) 0.0690(12) Uani 1 1 d . . . . .
H28A H 0.972990 0.670841 0.757822 0.104 Uiso 1 1 calc R U . . .
H28B H 1.019926 0.599583 0.693684 0.104 Uiso 1 1 calc R U . . .
H28C H 1.052466 0.576196 0.776256 0.104 Uiso 1 1 calc R U . . .
S2 S 0.77959(12) 0.56198(10) 0.55829(6) 0.0727(4) Uani 1 1 d . . . . .
O29 O 0.8773(3) 0.4963(3) 0.5783(3) 0.1146(16) Uani 1 1 d . . . . .
C30 C 0.8286(5) 0.6935(4) 0.5295(2) 0.0753(15) Uani 1 1 d . . . . .
C31 C 0.9034(5) 0.7379(5) 0.5855(3) 0.099(2) Uani 1 1 d . . . . .
H31A H 0.961616 0.688069 0.594250 0.149 Uiso 1 1 calc R U . . .
H31B H 0.864544 0.750027 0.630976 0.149 Uiso 1 1 calc R U . . .
H31C H 0.932888 0.804452 0.567891 0.149 Uiso 1 1 calc R U . . .
C32 C 0.8930(6) 0.6666(6) 0.4599(3) 0.130(3) Uani 1 1 d . . . . .
H32A H 0.845608 0.634145 0.424014 0.194 Uiso 1 1 calc R U . . .
H32B H 0.950481 0.617596 0.472233 0.194 Uiso 1 1 calc R U . . .
H32C H 0.923561 0.731054 0.439614 0.194 Uiso 1 1 calc R U . . .
C33 C 0.7356(6) 0.7615(6) 0.5123(4) 0.131(3) Uani 1 1 d . . . . .
H33A H 0.760469 0.826160 0.488910 0.196 Uiso 1 1 calc R U . . .
H33B H 0.697724 0.778941 0.557265 0.196 Uiso 1 1 calc R U . . .
H33C H 0.687397 0.724076 0.479290 0.196 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C2 2.024(3) . ?
Fe1 C22 2.025(3) . ?
Fe1 C1 2.029(3) . ?
Fe1 C21 2.032(3) . ?
Fe1 C24 2.038(3) . ?
Fe1 C4 2.040(3) . ?
Fe1 C3 2.049(3) . ?
Fe1 C23 2.049(3) . ?
Fe1 C5 2.060(3) . ?
Fe1 C25 2.062(3) . ?
C1 C2 1.423(5) . ?
C1 C5 1.444(4) . ?
C1 S1 1.771(3) . ?
C2 C3 1.400(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.411(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.429(4) . ?
C4 H4 0.9500 . ?
C5 Si1 1.883(3) . ?
Si1 C8 1.847(5) . ?
Si1 C6 1.858(7) . ?
Si1 C7 1.860(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
S1 O9 1.455(5) . ?
S1 C10B 1.844(5) . ?
S1 C10A 1.844(5) . ?
C10A C11A 1.40(2) . ?
C10A C13A 1.531(7) . ?
C10A C12A 1.64(2) . ?
C11A H11A 0.9800 . ?
C11A H11B 0.9800 . ?
C11A H11C 0.9800 . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9800 . ?
C13A H13B 0.9800 . ?
C13A H13C 0.9800 . ?
C10B C12B 1.40(2) . ?
C10B C13B 1.531(7) . ?
C10B C11B 1.65(3) . ?
C11B H11D 0.9800 . ?
C11B H11E 0.9800 . ?
C11B H11F 0.9800 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9799 . ?
C13B H13F 0.9796 . ?
C21 C22 1.422(5) . ?
C21 C25 1.446(4) . ?
C21 S2 1.770(3) . ?
C22 C23 1.420(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.426(4) . ?
C24 H24 0.9500 . ?
C25 Si2 1.883(3) . ?
Si2 C26 1.849(5) . ?
Si2 C28 1.850(4) . ?
Si2 C27 1.859(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
S2 O29 1.528(5) . ?
S2 C30 1.861(5) . ?
C30 C33 1.487(9) . ?
C30 C31 1.504(7) . ?
C30 C32 1.550(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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
C2 Fe1 C22 129.03(16) . . ?
C2 Fe1 C1 41.12(15) . . ?
C22 Fe1 C1 108.30(14) . . ?
C2 Fe1 C21 108.65(15) . . ?
C22 Fe1 C21 41.05(15) . . ?
C1 Fe1 C21 118.97(13) . . ?
C2 Fe1 C24 151.77(15) . . ?
C22 Fe1 C24 67.89(15) . . ?
C1 Fe1 C24 165.78(13) . . ?
C21 Fe1 C24 67.86(13) . . ?
C2 Fe1 C4 67.77(16) . . ?
C22 Fe1 C4 151.53(16) . . ?
C1 Fe1 C4 67.87(13) . . ?
C21 Fe1 C4 166.10(14) . . ?
C24 Fe1 C4 108.51(15) . . ?
C2 Fe1 C3 40.20(17) . . ?
C22 Fe1 C3 166.83(17) . . ?
C1 Fe1 C3 68.30(14) . . ?
C21 Fe1 C3 128.37(14) . . ?
C24 Fe1 C3 118.54(16) . . ?
C4 Fe1 C3 40.37(15) . . ?
C2 Fe1 C23 167.22(17) . . ?
C22 Fe1 C23 40.80(16) . . ?
C1 Fe1 C23 128.32(14) . . ?
C21 Fe1 C23 68.54(14) . . ?
C24 Fe1 C23 39.99(15) . . ?
C4 Fe1 C23 117.97(17) . . ?
C3 Fe1 C23 151.19(19) . . ?
C2 Fe1 C5 69.72(14) . . ?
C22 Fe1 C5 117.23(14) . . ?
C1 Fe1 C5 41.36(12) . . ?
C21 Fe1 C5 152.16(12) . . ?
C24 Fe1 C5 126.93(13) . . ?
C4 Fe1 C5 40.77(12) . . ?
C3 Fe1 C5 69.27(12) . . ?
C23 Fe1 C5 106.60(13) . . ?
C2 Fe1 C25 117.67(14) . . ?
C22 Fe1 C25 69.70(14) . . ?
C1 Fe1 C25 152.43(13) . . ?
C21 Fe1 C25 41.35(12) . . ?
C24 Fe1 C25 40.71(12) . . ?
C4 Fe1 C25 127.18(13) . . ?
C3 Fe1 C25 107.07(13) . . ?
C23 Fe1 C25 69.07(13) . . ?
C5 Fe1 C25 164.75(12) . . ?
C2 C1 C5 109.0(3) . . ?
C2 C1 S1 120.1(3) . . ?
C5 C1 S1 130.7(2) . . ?
C2 C1 Fe1 69.27(18) . . ?
C5 C1 Fe1 70.48(17) . . ?
S1 C1 Fe1 122.50(16) . . ?
C3 C2 C1 108.4(3) . . ?
C3 C2 Fe1 70.8(2) . . ?
C1 C2 Fe1 69.61(18) . . ?
C3 C2 H2 125.8 . . ?
C1 C2 H2 125.8 . . ?
Fe1 C2 H2 125.3 . . ?
C2 C3 C4 107.5(3) . . ?
C2 C3 Fe1 68.96(19) . . ?
C4 C3 Fe1 69.50(18) . . ?
C2 C3 H3 126.3 . . ?
C4 C3 H3 126.3 . . ?
Fe1 C3 H3 126.8 . . ?
C3 C4 C5 110.6(3) . . ?
C3 C4 Fe1 70.13(19) . . ?
C5 C4 Fe1 70.34(17) . . ?
C3 C4 H4 124.7 . . ?
C5 C4 H4 124.7 . . ?
Fe1 C4 H4 126.5 . . ?
C4 C5 C1 104.5(3) . . ?
C4 C5 Si1 120.0(2) . . ?
C1 C5 Si1 135.5(2) . . ?
C4 C5 Fe1 68.88(17) . . ?
C1 C5 Fe1 68.16(16) . . ?
Si1 C5 Fe1 125.93(15) . . ?
C8 Si1 C6 107.4(4) . . ?
C8 Si1 C7 109.4(2) . . ?
C6 Si1 C7 107.3(4) . . ?
C8 Si1 C5 115.9(2) . . ?
C6 Si1 C5 105.7(3) . . ?
C7 Si1 C5 110.70(19) . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O9 S1 C1 108.6(2) . . ?
O9 S1 C10B 108.1(3) . . ?
C1 S1 C10B 101.36(19) . . ?
O9 S1 C10A 108.1(3) . . ?
C1 S1 C10A 101.36(19) . . ?
C11A C10A C13A 121.4(9) . . ?
C11A C10A C12A 110.8(8) . . ?
C13A C10A C12A 102.4(8) . . ?
C11A C10A S1 114.3(7) . . ?
C13A C10A S1 103.7(4) . . ?
C12A C10A S1 101.9(7) . . ?
C10A C11A H11A 109.5 . . ?
C10A C11A H11B 109.5 . . ?
H11A C11A H11B 109.5 . . ?
C10A C11A H11C 109.5 . . ?
H11A C11A H11C 109.5 . . ?
H11B C11A H11C 109.5 . . ?
C10A C12A H12A 109.5 . . ?
C10A C12A H12B 109.5 . . ?
H12A C12A H12B 109.5 . . ?
C10A C12A H12C 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
C10A C13A H13A 109.5 . . ?
C10A C13A H13B 109.5 . . ?
H13A C13A H13B 109.5 . . ?
C10A C13A H13C 109.5 . . ?
H13A C13A H13C 109.5 . . ?
H13B C13A H13C 109.5 . . ?
C12B C10B C13B 117.7(10) . . ?
C12B C10B C11B 108.4(11) . . ?
C13B C10B C11B 101.7(9) . . ?
C12B C10B S1 121.2(10) . . ?
C13B C10B S1 103.7(4) . . ?
C11B C10B S1 101.3(7) . . ?
C10B C11B H11D 109.5 . . ?
C10B C11B H11E 109.5 . . ?
H11D C11B H11E 109.5 . . ?
C10B C11B H11F 109.5 . . ?
H11D C11B H11F 109.5 . . ?
H11E C11B H11F 109.5 . . ?
C10B C12B H12D 109.5 . . ?
C10B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C10B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C10B C13B H13D 109.4 . . ?
C10B C13B H13E 109.4 . . ?
H13D C13B H13E 109.5 . . ?
C10B C13B H13F 109.4 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C22 C21 C25 109.0(3) . . ?
C22 C21 S2 123.0(3) . . ?
C25 C21 S2 127.8(2) . . ?
C22 C21 Fe1 69.20(18) . . ?
C25 C21 Fe1 70.44(17) . . ?
S2 C21 Fe1 122.86(16) . . ?
C23 C22 C21 107.9(3) . . ?
C23 C22 Fe1 70.51(19) . . ?
C21 C22 Fe1 69.74(18) . . ?
C23 C22 H22 126.1 . . ?
C21 C22 H22 126.1 . . ?
Fe1 C22 H22 125.3 . . ?
C24 C23 C22 107.3(3) . . ?
C24 C23 Fe1 69.59(18) . . ?
C22 C23 Fe1 68.69(19) . . ?
C24 C23 H23 126.4 . . ?
C22 C23 H23 126.4 . . ?
Fe1 C23 H23 126.9 . . ?
C23 C24 C25 111.2(3) . . ?
C23 C24 Fe1 70.4(2) . . ?
C25 C24 Fe1 70.54(17) . . ?
C23 C24 H24 124.4 . . ?
C25 C24 H24 124.4 . . ?
Fe1 C24 H24 126.3 . . ?
C24 C25 C21 104.6(3) . . ?
C24 C25 Si2 120.8(2) . . ?
C21 C25 Si2 134.6(2) . . ?
C24 C25 Fe1 68.75(17) . . ?
C21 C25 Fe1 68.21(16) . . ?
Si2 C25 Fe1 126.43(15) . . ?
C26 Si2 C28 110.0(3) . . ?
C26 Si2 C27 106.3(4) . . ?
C28 Si2 C27 107.5(3) . . ?
C26 Si2 C25 115.9(2) . . ?
C28 Si2 C25 111.09(18) . . ?
C27 Si2 C25 105.4(2) . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O29 S2 C21 105.5(2) . . ?
O29 S2 C30 107.2(3) . . ?
C21 S2 C30 101.24(19) . . ?
C33 C30 C31 114.6(6) . . ?
C33 C30 C32 111.2(5) . . ?
C31 C30 C32 108.9(5) . . ?
C33 C30 S2 109.0(4) . . ?
C31 C30 S2 110.4(4) . . ?
C32 C30 S2 102.0(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

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
C5 C1 C2 C3 1.1(4) . . . . ?
S1 C1 C2 C3 176.9(2) . . . . ?
Fe1 C1 C2 C3 60.5(2) . . . . ?
C5 C1 C2 Fe1 -59.4(2) . . . . ?
S1 C1 C2 Fe1 116.4(2) . . . . ?
C1 C2 C3 C4 -0.7(4) . . . . ?
Fe1 C2 C3 C4 59.0(2) . . . . ?
C1 C2 C3 Fe1 -59.7(2) . . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
Fe1 C3 C4 C5 58.8(2) . . . . ?
C2 C3 C4 Fe1 -58.7(2) . . . . ?
C3 C4 C5 C1 0.6(3) . . . . ?
Fe1 C4 C5 C1 59.22(19) . . . . ?
C3 C4 C5 Si1 -178.9(2) . . . . ?
Fe1 C4 C5 Si1 -120.2(2) . . . . ?
C3 C4 C5 Fe1 -58.7(2) . . . . ?
C2 C1 C5 C4 -1.0(3) . . . . ?
S1 C1 C5 C4 -176.2(3) . . . . ?
Fe1 C1 C5 C4 -59.70(19) . . . . ?
C2 C1 C5 Si1 178.3(2) . . . . ?
S1 C1 C5 Si1 3.1(5) . . . . ?
Fe1 C1 C5 Si1 119.6(3) . . . . ?
C2 C1 C5 Fe1 58.7(2) . . . . ?
S1 C1 C5 Fe1 -116.5(3) . . . . ?
C4 C5 Si1 C8 138.7(3) . . . . ?
C1 C5 Si1 C8 -40.5(4) . . . . ?
Fe1 C5 Si1 C8 54.2(3) . . . . ?
C4 C5 Si1 C6 19.9(4) . . . . ?
C1 C5 Si1 C6 -159.3(4) . . . . ?
Fe1 C5 Si1 C6 -64.6(4) . . . . ?
C4 C5 Si1 C7 -95.9(4) . . . . ?
C1 C5 Si1 C7 84.8(4) . . . . ?
Fe1 C5 Si1 C7 179.5(3) . . . . ?
C2 C1 S1 O9 -159.6(3) . . . . ?
C5 C1 S1 O9 15.2(4) . . . . ?
Fe1 C1 S1 O9 -76.2(3) . . . . ?
C2 C1 S1 C10B 86.7(3) . . . . ?
C5 C1 S1 C10B -98.5(4) . . . . ?
Fe1 C1 S1 C10B 170.0(3) . . . . ?
C2 C1 S1 C10A 86.7(3) . . . . ?
C5 C1 S1 C10A -98.5(4) . . . . ?
Fe1 C1 S1 C10A 170.0(3) . . . . ?
O9 S1 C10A C11A -166.4(10) . . . . ?
C1 S1 C10A C11A -52.4(10) . . . . ?
O9 S1 C10A C13A 59.2(5) . . . . ?
C1 S1 C10A C13A 173.3(5) . . . . ?
O9 S1 C10A C12A -46.9(8) . . . . ?
C1 S1 C10A C12A 67.2(8) . . . . ?
O9 S1 C10B C12B -75.8(13) . . . . ?
C1 S1 C10B C12B 38.3(13) . . . . ?
O9 S1 C10B C13B 59.2(5) . . . . ?
C1 S1 C10B C13B 173.3(5) . . . . ?
O9 S1 C10B C11B 164.4(8) . . . . ?
C1 S1 C10B C11B -81.5(8) . . . . ?
C25 C21 C22 C23 1.1(4) . . . . ?
S2 C21 C22 C23 176.9(2) . . . . ?
Fe1 C21 C22 C23 60.5(2) . . . . ?
C25 C21 C22 Fe1 -59.3(2) . . . . ?
S2 C21 C22 Fe1 116.5(2) . . . . ?
C21 C22 C23 C24 -0.9(4) . . . . ?
Fe1 C22 C23 C24 59.1(2) . . . . ?
C21 C22 C23 Fe1 -60.0(2) . . . . ?
C22 C23 C24 C25 0.3(4) . . . . ?
Fe1 C23 C24 C25 58.8(2) . . . . ?
C22 C23 C24 Fe1 -58.6(2) . . . . ?
C23 C24 C25 C21 0.4(3) . . . . ?
Fe1 C24 C25 C21 59.2(2) . . . . ?
C23 C24 C25 Si2 -179.4(2) . . . . ?
Fe1 C24 C25 Si2 -120.7(2) . . . . ?
C23 C24 C25 Fe1 -58.8(2) . . . . ?
C22 C21 C25 C24 -0.9(3) . . . . ?
S2 C21 C25 C24 -176.5(2) . . . . ?
Fe1 C21 C25 C24 -59.5(2) . . . . ?
C22 C21 C25 Si2 178.8(2) . . . . ?
S2 C21 C25 Si2 3.3(5) . . . . ?
Fe1 C21 C25 Si2 120.3(3) . . . . ?
C22 C21 C25 Fe1 58.6(2) . . . . ?
S2 C21 C25 Fe1 -116.9(3) . . . . ?
C24 C25 Si2 C26 125.7(4) . . . . ?
C21 C25 Si2 C26 -54.0(4) . . . . ?
Fe1 C25 Si2 C26 40.6(4) . . . . ?
C24 C25 Si2 C28 -107.7(3) . . . . ?
C21 C25 Si2 C28 72.5(4) . . . . ?
Fe1 C25 Si2 C28 167.1(2) . . . . ?
C24 C25 Si2 C27 8.5(4) . . . . ?
C21 C25 Si2 C27 -171.3(4) . . . . ?
Fe1 C25 Si2 C27 -76.7(3) . . . . ?
C22 C21 S2 O29 -169.3(3) . . . . ?
C25 C21 S2 O29 5.7(3) . . . . ?
Fe1 C21 S2 O29 -84.1(3) . . . . ?
C22 C21 S2 C30 79.1(3) . . . . ?
C25 C21 S2 C30 -105.9(3) . . . . ?
Fe1 C21 S2 C30 164.3(2) . . . . ?
O29 S2 C30 C33 -177.8(5) . . . . ?
C21 S2 C30 C33 -67.6(5) . . . . ?
O29 S2 C30 C31 -51.1(5) . . . . ?
C21 S2 C30 C31 59.2(5) . . . . ?
O29 S2 C30 C32 64.5(5) . . . . ?
C21 S2 C30 C32 174.8(4) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: job.res
#...............................................................................


####################################################################### 
# 
# 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_MW5462
_database_code_depnum_ccdc_archive 'CCDC 2204522'
loop_
_audit_author_name
_audit_author_address
'Thierry Roisnel'
;ISCR
France
;
_audit_update_record             
;
2022-08-30 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;

#------------------------------------------------------------------------------#
# Date of experiment: 31 janvier 2022                                          #
#------------------------------------------------------------------------------#


#------------------------------------------------------------------------------#
#                             CHEMICAL INFORMATION                             #
#------------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H41 Fe I O2 S2 Si2'
_chemical_formula_sum            'C24 H41 Fe I O2 S2 Si2'
_chemical_formula_weight         664.62
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#------------------------------------------------------------------------------#
#                    SPACE GROUP AND UNIT CELL INFORMATION                     #
#------------------------------------------------------------------------------#

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'
_space_group_IT_number           4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   11.8827(7)
_cell_length_b                   11.1068(5)
_cell_length_c                   13.1403(7)
_cell_angle_alpha                90
_cell_angle_beta                 94.755(2)
_cell_angle_gamma                90
_cell_volume                     1728.27(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4566
_cell_measurement_theta_min      2.2211
_cell_measurement_theta_max      23.6496
_cell_measurement_wavelength     0.710730


#------------------------------------------------------------------------------#
#                              ORIENTATION MATRIX                              #
#------------------------------------------------------------------------------#

_diffrn_orient_matrix_UB_11      0.0455266
_diffrn_orient_matrix_UB_21      0.0709229
_diffrn_orient_matrix_UB_31      0.0053377
_diffrn_orient_matrix_UB_12      0.0114340
_diffrn_orient_matrix_UB_22      -0.0139780
_diffrn_orient_matrix_UB_32      0.0882054
_diffrn_orient_matrix_UB_13      0.0667748
_diffrn_orient_matrix_UB_23      -0.0342670
_diffrn_orient_matrix_UB_33      -0.0140863


#------------------------------------------------------------------------------#
#                             CRYSTAL INFORMATION                              #
#------------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.260
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             680
_exptl_special_details           
;
 ?
;

#------------------------------------------------------------------------------#
#                            ABSORPTION CORRECTION                             #
#------------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_T_max  0.671

#------------------------------------------------------------------------------#
#                               DATA COLLECTION                                #
#------------------------------------------------------------------------------#

# Software                   : BIS 2014.5.0.0/23-May-2014 && APEX2_2014.11-0   #
# Number of scans            :        3                                        #
# Total number of frames     :      332                                        #
# Total length of scans      :   332.00 (deg.)                                 #
# Rotation speed             :    30.00 sec./deg.                              #
# Total exposition time      :      2 h  46.0 min.                             #
#                                                                              #
#    Scan  Time(s) Width DX(mm) Frames Range 2Theta  Omega    Phi    Chi  T(K) #
#..............................................................................#
#                                                                              #
#  1 Omega   30.0  1.00    35.0   105  105.0   16.0   14.8  287.3  -51.9 296.1 #
#  2 Omega   30.0  1.00    35.0   125  125.0   16.0  332.0  140.2   -2.2 296.1 #
#  3 Omega   30.0  1.00    35.0   102  102.0   16.0   14.5   64.4  -45.8 296.1 #
#                                                                              #
#..............................................................................#

_diffrn_measurement_device_type  'APEXII Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 CCD-LDI-APEX2
_diffrn_detector_area_resol_mean 8.33
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_source_power             50.0
_diffrn_reflns_av_uneti/neti     0.0440
_diffrn_reflns_av_r_equivalents  0.0248
_diffrn_reflns_number            13763
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.881
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             6772
_reflns_number_gt                4723
_reflns_threshold_expression     >2sigma(I)
_reflns_Friedel_coverage         0.627
_reflns_Friedel_fraction_max     0.691
_reflns_Friedel_fraction_full    0.748

_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.
;

#------------------------------------------------------------------------------#
#                            COMPUTER PROGRAMS USED                            #
#------------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_molecular_graphics    
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2021)'

#------------------------------------------------------------------------------#
#                            REFINEMENT INFORMATION                            #
#------------------------------------------------------------------------------#

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0604P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6772
_refine_ls_number_parameters     302
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.1079
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details 
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(2)

#------------------------------------------------------------------------------#
#               ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS               #
#------------------------------------------------------------------------------#

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.62593(7) 0.44065(7) 0.23776(6) 0.0450(2) Uani 1 1 d . . . . .
I1 I 0.49771(5) 0.72636(5) 0.14639(5) 0.1002(3) Uani 1 1 d . . . . .
C1 C 0.6317(5) 0.4884(6) 0.3929(5) 0.0550(16) Uani 1 1 d . . . . .
C2 C 0.5428(6) 0.5508(7) 0.3314(6) 0.0619(17) Uani 1 1 d . . . . .
H2 H 0.466498 0.546650 0.342084 0.074 Uiso 1 1 calc R U . . .
C3 C 0.5875(6) 0.6186(6) 0.2530(6) 0.0596(19) Uani 1 1 d . . . . .
C4 C 0.7065(6) 0.6023(6) 0.2594(5) 0.0569(17) Uani 1 1 d . . . . .
H4 H 0.756318 0.634399 0.215591 0.068 Uiso 1 1 calc R U . . .
C5 C 0.7350(5) 0.5270(5) 0.3460(5) 0.0468(14) Uani 1 1 d . . . . .
Si1 Si 0.6025(2) 0.3946(2) 0.50436(16) 0.0700(6) Uani 1 1 d . . . . .
C6 C 0.6384(12) 0.4820(13) 0.6235(7) 0.147(6) Uani 1 1 d . . . . .
H6A H 0.633348 0.566588 0.608627 0.221 Uiso 1 1 calc R U . . .
H6B H 0.713957 0.462791 0.650149 0.221 Uiso 1 1 calc R U . . .
H6C H 0.586575 0.461846 0.673079 0.221 Uiso 1 1 calc R U . . .
C7 C 0.4461(8) 0.3750(10) 0.4966(9) 0.112(3) Uani 1 1 d . . . . .
H7A H 0.410241 0.447146 0.469938 0.168 Uiso 1 1 calc R U . . .
H7B H 0.422791 0.359174 0.563485 0.168 Uiso 1 1 calc R U . . .
H7C H 0.424916 0.308639 0.452267 0.168 Uiso 1 1 calc R U . . .
C8 C 0.6638(8) 0.2394(9) 0.5089(8) 0.099(3) Uani 1 1 d . . . . .
H8A H 0.610985 0.184440 0.474733 0.148 Uiso 1 1 calc R U . . .
H8B H 0.679262 0.215053 0.578733 0.148 Uiso 1 1 calc R U . . .
H8C H 0.732671 0.239138 0.475490 0.148 Uiso 1 1 calc R U . . .
S1 S 0.87415(14) 0.47808(15) 0.38523(13) 0.0568(4) Uani 1 1 d . . . . .
O9 O 0.8632(5) 0.3986(5) 0.4727(4) 0.0820(16) Uani 1 1 d . . . . .
C10 C 0.9379(7) 0.6204(7) 0.4366(6) 0.074(2) Uani 1 1 d . . . . .
C11 C 1.0491(8) 0.5809(9) 0.4905(8) 0.110(4) Uani 1 1 d . . . . .
H11A H 1.091613 0.650422 0.513987 0.165 Uiso 1 1 calc R U . . .
H11B H 1.091197 0.536120 0.443964 0.165 Uiso 1 1 calc R U . . .
H11C H 1.035096 0.530956 0.547732 0.165 Uiso 1 1 calc R U . . .
C12 C 0.9646(8) 0.7012(9) 0.3503(7) 0.101(3) Uani 1 1 d . . . . .
H12A H 0.898565 0.746645 0.327392 0.152 Uiso 1 1 calc R U . . .
H12B H 0.987974 0.653392 0.295004 0.152 Uiso 1 1 calc R U . . .
H12C H 1.024301 0.755394 0.373410 0.152 Uiso 1 1 calc R U . . .
C13 C 0.8675(10) 0.6768(12) 0.5106(11) 0.150(6) Uani 1 1 d . . . . .
H13A H 0.913221 0.729837 0.554461 0.224 Uiso 1 1 calc R U . . .
H13B H 0.835704 0.615451 0.550940 0.224 Uiso 1 1 calc R U . . .
H13C H 0.807851 0.721910 0.474651 0.224 Uiso 1 1 calc R U . . .
C21 C 0.6730(6) 0.3653(6) 0.1027(5) 0.0552(17) Uani 1 1 d . . . . .
C22 C 0.5535(6) 0.3917(7) 0.0974(5) 0.0626(19) Uani 1 1 d . . . . .
H22 H 0.516020 0.442922 0.049851 0.075 Uiso 1 1 calc R U . . .
C23 C 0.5016(6) 0.3291(7) 0.1742(6) 0.066(2) Uani 1 1 d . . . . .
H23 H 0.425576 0.332106 0.185904 0.080 Uiso 1 1 calc R U . . .
C24 C 0.5858(6) 0.2612(6) 0.2302(6) 0.0592(18) Uani 1 1 d . . . . .
H24 H 0.575430 0.211299 0.285516 0.071 Uiso 1 1 calc R U . . .
C25 C 0.6888(5) 0.2827(5) 0.1869(5) 0.0483(14) Uani 1 1 d . . . . .
Si2 Si 0.7690(2) 0.4336(2) 0.01005(15) 0.0781(6) Uani 1 1 d . . . . .
C26 C 0.8322(8) 0.3147(10) -0.0720(7) 0.106(4) Uani 1 1 d . . . . .
H26A H 0.863749 0.352756 -0.128744 0.160 Uiso 1 1 calc R U . . .
H26B H 0.774351 0.259242 -0.096780 0.160 Uiso 1 1 calc R U . . .
H26C H 0.890517 0.272040 -0.031887 0.160 Uiso 1 1 calc R U . . .
C28 C 0.6707(9) 0.5350(10) -0.0720(7) 0.108(3) Uani 1 1 d . . . . .
H28A H 0.644938 0.599326 -0.031023 0.162 Uiso 1 1 calc R U . . .
H28B H 0.607085 0.489190 -0.100218 0.162 Uiso 1 1 calc R U . . .
H28C H 0.710298 0.567932 -0.126422 0.162 Uiso 1 1 calc R U . . .
C27 C 0.8881(9) 0.5266(11) 0.0684(8) 0.110(4) Uani 1 1 d . . . . .
H27A H 0.891762 0.519161 0.141419 0.165 Uiso 1 1 calc R U . . .
H27B H 0.876196 0.609363 0.049570 0.165 Uiso 1 1 calc R U . . .
H27C H 0.957754 0.498994 0.044358 0.165 Uiso 1 1 calc R U . . .
S2 S 0.82053(14) 0.21707(19) 0.23041(13) 0.0595(4) Uani 1 1 d . . . . .
O29 O 0.9040(4) 0.2711(6) 0.1668(5) 0.0886(17) Uani 1 1 d . . . . .
C30 C 0.7977(8) 0.0578(7) 0.1884(6) 0.075(2) Uani 1 1 d . . . . .
C31 C 0.7290(8) -0.0029(7) 0.2659(7) 0.087(3) Uani 1 1 d . . . . .
H31A H 0.659423 0.039920 0.270138 0.131 Uiso 1 1 calc R U . . .
H31B H 0.771086 -0.002705 0.331509 0.131 Uiso 1 1 calc R U . . .
H31C H 0.713102 -0.084446 0.245132 0.131 Uiso 1 1 calc R U . . .
C32 C 0.7373(13) 0.0537(9) 0.0803(8) 0.137(5) Uani 1 1 d . . . . .
H32A H 0.746078 -0.024807 0.051449 0.205 Uiso 1 1 calc R U . . .
H32B H 0.769740 0.112922 0.038196 0.205 Uiso 1 1 calc R U . . .
H32C H 0.658483 0.070548 0.083686 0.205 Uiso 1 1 calc R U . . .
C33 C 0.9163(9) 0.0047(10) 0.1929(8) 0.113(4) Uani 1 1 d . . . . .
H33A H 0.951170 0.011188 0.261215 0.169 Uiso 1 1 calc R U . . .
H33B H 0.960375 0.047895 0.147007 0.169 Uiso 1 1 calc R U . . .
H33C H 0.911896 -0.078588 0.173287 0.169 Uiso 1 1 calc R U . . .



#------------------------------------------------------------------------------#
#                              MOLECULAR GEOMETRY                              #
#------------------------------------------------------------------------------#

_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 C25 2.041(6) . ?
Fe1 C3 2.042(7) . ?
Fe1 C4 2.043(7) . ?
Fe1 C22 2.044(6) . ?
Fe1 C2 2.046(7) . ?
Fe1 C24 2.050(7) . ?
Fe1 C23 2.051(7) . ?
Fe1 C5 2.077(6) . ?
Fe1 C21 2.081(7) . ?
Fe1 C1 2.102(7) . ?
I1 C3 2.070(7) . ?
C1 C2 1.452(9) . ?
C1 C5 1.482(9) . ?
C1 Si1 1.853(7) . ?
C2 C3 1.414(11) . ?
C2 H2 0.9300 . ?
C3 C4 1.422(10) . ?
C4 C5 1.430(9) . ?
C4 H4 0.9300 . ?
C5 S1 1.776(6) . ?
Si1 C6 1.861(10) . ?
Si1 C7 1.865(10) . ?
Si1 C8 1.870(10) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
S1 O9 1.463(5) . ?
S1 C10 1.855(8) . ?
C10 C13 1.474(14) . ?
C10 C12 1.500(12) . ?
C10 C11 1.511(11) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C21 C25 1.438(9) . ?
C21 C22 1.446(10) . ?
C21 Si2 1.894(7) . ?
C22 C23 1.409(11) . ?
C22 H22 0.9300 . ?
C23 C24 1.411(11) . ?
C23 H23 0.9300 . ?
C24 C25 1.412(9) . ?
C24 H24 0.9300 . ?
C25 S2 1.778(6) . ?
Si2 C27 1.865(9) . ?
Si2 C28 1.894(10) . ?
Si2 C26 1.898(10) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
S2 O29 1.476(6) . ?
S2 C30 1.867(8) . ?
C30 C31 1.515(12) . ?
C30 C33 1.524(12) . ?
C30 C32 1.539(13) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?

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
C25 Fe1 C3 162.8(3) . . ?
C25 Fe1 C4 128.4(3) . . ?
C3 Fe1 C4 40.7(3) . . ?
C25 Fe1 C22 67.3(3) . . ?
C3 Fe1 C22 105.4(3) . . ?
C4 Fe1 C22 121.1(3) . . ?
C25 Fe1 C2 156.7(3) . . ?
C3 Fe1 C2 40.5(3) . . ?
C4 Fe1 C2 68.6(3) . . ?
C22 Fe1 C2 120.9(3) . . ?
C25 Fe1 C24 40.4(3) . . ?
C3 Fe1 C24 153.2(3) . . ?
C4 Fe1 C24 164.9(3) . . ?
C22 Fe1 C24 67.6(3) . . ?
C2 Fe1 C24 119.2(3) . . ?
C25 Fe1 C23 67.6(3) . . ?
C3 Fe1 C23 117.7(3) . . ?
C4 Fe1 C23 154.2(3) . . ?
C22 Fe1 C23 40.2(3) . . ?
C2 Fe1 C23 103.8(3) . . ?
C24 Fe1 C23 40.2(3) . . ?
C25 Fe1 C5 113.3(2) . . ?
C3 Fe1 C5 67.6(3) . . ?
C4 Fe1 C5 40.6(2) . . ?
C22 Fe1 C5 158.9(3) . . ?
C2 Fe1 C5 67.5(3) . . ?
C24 Fe1 C5 127.7(3) . . ?
C23 Fe1 C5 160.8(3) . . ?
C25 Fe1 C21 40.8(3) . . ?
C3 Fe1 C21 123.5(3) . . ?
C4 Fe1 C21 108.4(3) . . ?
C22 Fe1 C21 41.0(3) . . ?
C2 Fe1 C21 158.5(3) . . ?
C24 Fe1 C21 69.2(3) . . ?
C23 Fe1 C21 69.2(3) . . ?
C5 Fe1 C21 125.0(3) . . ?
C25 Fe1 C1 123.4(2) . . ?
C3 Fe1 C1 69.5(3) . . ?
C4 Fe1 C1 70.5(3) . . ?
C22 Fe1 C1 156.9(3) . . ?
C2 Fe1 C1 40.9(3) . . ?
C24 Fe1 C1 106.3(3) . . ?
C23 Fe1 C1 120.8(3) . . ?
C5 Fe1 C1 41.5(2) . . ?
C21 Fe1 C1 160.0(2) . . ?
C2 C1 C5 102.7(6) . . ?
C2 C1 Si1 122.2(5) . . ?
C5 C1 Si1 135.0(5) . . ?
C2 C1 Fe1 67.4(4) . . ?
C5 C1 Fe1 68.3(3) . . ?
Si1 C1 Fe1 129.1(3) . . ?
C3 C2 C1 111.1(6) . . ?
C3 C2 Fe1 69.6(4) . . ?
C1 C2 Fe1 71.6(4) . . ?
C3 C2 H2 124.5 . . ?
C1 C2 H2 124.5 . . ?
Fe1 C2 H2 125.9 . . ?
C2 C3 C4 108.7(6) . . ?
C2 C3 Fe1 69.9(4) . . ?
C4 C3 Fe1 69.7(4) . . ?
C2 C3 I1 126.7(5) . . ?
C4 C3 I1 124.6(6) . . ?
Fe1 C3 I1 126.9(4) . . ?
C3 C4 C5 106.8(7) . . ?
C3 C4 Fe1 69.6(4) . . ?
C5 C4 Fe1 71.0(4) . . ?
C3 C4 H4 126.6 . . ?
C5 C4 H4 126.6 . . ?
Fe1 C4 H4 124.5 . . ?
C4 C5 C1 110.5(6) . . ?
C4 C5 S1 124.3(5) . . ?
C1 C5 S1 125.0(5) . . ?
C4 C5 Fe1 68.4(3) . . ?
C1 C5 Fe1 70.1(3) . . ?
S1 C5 Fe1 124.8(3) . . ?
C1 Si1 C6 109.0(4) . . ?
C1 Si1 C7 105.9(4) . . ?
C6 Si1 C7 105.4(6) . . ?
C1 Si1 C8 116.4(4) . . ?
C6 Si1 C8 113.1(6) . . ?
C7 Si1 C8 106.2(5) . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7A 109.5 . . ?
Si1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O9 S1 C5 105.7(3) . . ?
O9 S1 C10 106.8(3) . . ?
C5 S1 C10 100.8(3) . . ?
C13 C10 C12 114.3(10) . . ?
C13 C10 C11 109.6(9) . . ?
C12 C10 C11 107.3(8) . . ?
C13 C10 S1 111.4(6) . . ?
C12 C10 S1 109.9(6) . . ?
C11 C10 S1 103.8(6) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C25 C21 C22 103.4(6) . . ?
C25 C21 Si2 134.7(5) . . ?
C22 C21 Si2 122.0(5) . . ?
C25 C21 Fe1 68.1(4) . . ?
C22 C21 Fe1 68.1(4) . . ?
Si2 C21 Fe1 127.3(3) . . ?
C23 C22 C21 110.6(6) . . ?
C23 C22 Fe1 70.2(4) . . ?
C21 C22 Fe1 70.8(3) . . ?
C23 C22 H22 124.7 . . ?
C21 C22 H22 124.7 . . ?
Fe1 C22 H22 125.9 . . ?
C22 C23 C24 107.7(6) . . ?
C22 C23 Fe1 69.6(4) . . ?
C24 C23 Fe1 69.8(4) . . ?
C22 C23 H23 126.1 . . ?
C24 C23 H23 126.1 . . ?
Fe1 C23 H23 126.0 . . ?
C23 C24 C25 107.4(6) . . ?
C23 C24 Fe1 69.9(4) . . ?
C25 C24 Fe1 69.5(4) . . ?
C23 C24 H24 126.3 . . ?
C25 C24 H24 126.3 . . ?
Fe1 C24 H24 125.9 . . ?
C24 C25 C21 110.9(6) . . ?
C24 C25 S2 124.8(5) . . ?
C21 C25 S2 124.4(5) . . ?
C24 C25 Fe1 70.2(4) . . ?
C21 C25 Fe1 71.1(4) . . ?
S2 C25 Fe1 125.7(3) . . ?
C27 Si2 C28 108.4(5) . . ?
C27 Si2 C21 115.8(4) . . ?
C28 Si2 C21 103.2(4) . . ?
C27 Si2 C26 107.2(5) . . ?
C28 Si2 C26 110.2(5) . . ?
C21 Si2 C26 112.0(4) . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C28 H28A 109.5 . . ?
Si2 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si2 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si2 C27 H27A 109.5 . . ?
Si2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O29 S2 C25 105.4(3) . . ?
O29 S2 C30 107.8(4) . . ?
C25 S2 C30 101.0(3) . . ?
C31 C30 C33 110.5(8) . . ?
C31 C30 C32 111.8(9) . . ?
C33 C30 C32 112.5(8) . . ?
C31 C30 S2 107.2(5) . . ?
C33 C30 S2 104.1(7) . . ?
C32 C30 S2 110.2(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

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
C5 C1 C2 C3 1.2(7) . . . . ?
Si1 C1 C2 C3 178.3(5) . . . . ?
Fe1 C1 C2 C3 -58.5(5) . . . . ?
C5 C1 C2 Fe1 59.8(4) . . . . ?
Si1 C1 C2 Fe1 -123.1(5) . . . . ?
C1 C2 C3 C4 0.7(8) . . . . ?
Fe1 C2 C3 C4 -59.0(5) . . . . ?
C1 C2 C3 Fe1 59.7(5) . . . . ?
C1 C2 C3 I1 -178.7(5) . . . . ?
Fe1 C2 C3 I1 121.6(5) . . . . ?
C2 C3 C4 C5 -2.4(8) . . . . ?
Fe1 C3 C4 C5 -61.6(4) . . . . ?
I1 C3 C4 C5 177.0(5) . . . . ?
C2 C3 C4 Fe1 59.2(5) . . . . ?
I1 C3 C4 Fe1 -121.4(5) . . . . ?
C3 C4 C5 C1 3.2(7) . . . . ?
Fe1 C4 C5 C1 -57.4(4) . . . . ?
C3 C4 C5 S1 178.9(5) . . . . ?
Fe1 C4 C5 S1 118.3(5) . . . . ?
C3 C4 C5 Fe1 60.7(4) . . . . ?
C2 C1 C5 C4 -2.7(7) . . . . ?
Si1 C1 C5 C4 -179.3(5) . . . . ?
Fe1 C1 C5 C4 56.4(4) . . . . ?
C2 C1 C5 S1 -178.4(5) . . . . ?
Si1 C1 C5 S1 5.1(9) . . . . ?
Fe1 C1 C5 S1 -119.2(5) . . . . ?
C2 C1 C5 Fe1 -59.2(4) . . . . ?
Si1 C1 C5 Fe1 124.3(6) . . . . ?
C2 C1 Si1 C6 -100.9(7) . . . . ?
C5 C1 Si1 C6 75.1(8) . . . . ?
Fe1 C1 Si1 C6 173.2(6) . . . . ?
C2 C1 Si1 C7 12.0(7) . . . . ?
C5 C1 Si1 C7 -172.0(7) . . . . ?
Fe1 C1 Si1 C7 -73.9(6) . . . . ?
C2 C1 Si1 C8 129.7(6) . . . . ?
C5 C1 Si1 C8 -54.3(8) . . . . ?
Fe1 C1 Si1 C8 43.8(6) . . . . ?
C4 C5 S1 O9 -177.1(5) . . . . ?
C1 C5 S1 O9 -2.0(6) . . . . ?
Fe1 C5 S1 O9 -91.0(4) . . . . ?
C4 C5 S1 C10 71.9(6) . . . . ?
C1 C5 S1 C10 -113.0(6) . . . . ?
Fe1 C5 S1 C10 158.0(4) . . . . ?
O9 S1 C10 C13 -59.0(9) . . . . ?
C5 S1 C10 C13 51.3(9) . . . . ?
O9 S1 C10 C12 173.3(6) . . . . ?
C5 S1 C10 C12 -76.5(7) . . . . ?
O9 S1 C10 C11 58.9(7) . . . . ?
C5 S1 C10 C11 169.1(6) . . . . ?
C25 C21 C22 C23 0.3(7) . . . . ?
Si2 C21 C22 C23 179.7(5) . . . . ?
Fe1 C21 C22 C23 -59.1(5) . . . . ?
C25 C21 C22 Fe1 59.4(4) . . . . ?
Si2 C21 C22 Fe1 -121.3(5) . . . . ?
C21 C22 C23 C24 -0.2(8) . . . . ?
Fe1 C22 C23 C24 -59.6(5) . . . . ?
C21 C22 C23 Fe1 59.5(5) . . . . ?
C22 C23 C24 C25 -0.1(8) . . . . ?
Fe1 C23 C24 C25 -59.6(5) . . . . ?
C22 C23 C24 Fe1 59.5(5) . . . . ?
C23 C24 C25 C21 0.3(8) . . . . ?
Fe1 C24 C25 C21 -59.6(5) . . . . ?
C23 C24 C25 S2 -179.8(5) . . . . ?
Fe1 C24 C25 S2 120.3(5) . . . . ?
C23 C24 C25 Fe1 59.9(5) . . . . ?
C22 C21 C25 C24 -0.4(7) . . . . ?
Si2 C21 C25 C24 -179.6(5) . . . . ?
Fe1 C21 C25 C24 59.0(5) . . . . ?
C22 C21 C25 S2 179.7(5) . . . . ?
Si2 C21 C25 S2 0.5(9) . . . . ?
Fe1 C21 C25 S2 -120.9(5) . . . . ?
C22 C21 C25 Fe1 -59.4(4) . . . . ?
Si2 C21 C25 Fe1 121.4(6) . . . . ?
C25 C21 Si2 C27 -60.6(8) . . . . ?
C22 C21 Si2 C27 120.4(7) . . . . ?
Fe1 C21 Si2 C27 34.8(7) . . . . ?
C25 C21 Si2 C28 -178.8(7) . . . . ?
C22 C21 Si2 C28 2.1(7) . . . . ?
Fe1 C21 Si2 C28 -83.5(5) . . . . ?
C25 C21 Si2 C26 62.8(7) . . . . ?
C22 C21 Si2 C26 -116.3(6) . . . . ?
Fe1 C21 Si2 C26 158.1(5) . . . . ?
C24 C25 S2 O29 -176.6(6) . . . . ?
C21 C25 S2 O29 3.3(6) . . . . ?
Fe1 C25 S2 O29 -87.2(5) . . . . ?
C24 C25 S2 C30 71.2(6) . . . . ?
C21 C25 S2 C30 -108.9(6) . . . . ?
Fe1 C25 S2 C30 160.6(4) . . . . ?
O29 S2 C30 C31 169.9(6) . . . . ?
C25 S2 C30 C31 -79.7(6) . . . . ?
O29 S2 C30 C33 52.8(7) . . . . ?
C25 S2 C30 C33 163.2(6) . . . . ?
O29 S2 C30 C32 -68.1(8) . . . . ?
C25 S2 C30 C32 42.2(8) . . . . ?

#------------------------------------------------------------------------------#
#                                EMBEDDED FILES                                #
#------------------------------------------------------------------------------#
#                                                                              #

#...............................................................................
# .RES SHELXL file: sqz.res
#...............................................................................



# ............... End of .HKL file ........................................... #
#------------------------------------------------------------------------------#

#...............................................................................
# .FAB SHELXL file: sqz.fab
#...............................................................................


