# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_date             2013-01-14T11:38:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H8 Cl8 Fe2 S8, 4(H2 O), C3 H6 O'
_chemical_formula_sum            'C27 H22 Cl8 Fe2 O5 S8'
_chemical_formula_weight         1078.23
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.590(2)
_cell_length_b                   10.8710(10)
_cell_length_c                   14.426(4)
_cell_angle_alpha                68.868(17)
_cell_angle_beta                 82.287(18)
_cell_angle_gamma                74.817(8)
_cell_volume                     1493.6(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    70
_cell_measurement_theta_min      3
_cell_measurement_theta_max      20
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            'dark violet'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
19 -1 0 0.075
1 6 4 0.209
-16 -1 -1 0.125
1 -16 -11 0.233
-1 -1 8 0.046
1 1 -9 0.074

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.534
_exptl_absorpt_correction_T_max  0.718

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.1155
_diffrn_reflns_av_unetI/netI     0.1313
_diffrn_reflns_number            31995
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             6825
_reflns_number_gt                3739
_reflns_threshold_expression     >2σ(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   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 > 2σ(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)+(0.0500P)²+15.0000P] where P=(Fo²+2Fc²)/3"
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6825
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.2339
_refine_ls_wR_factor_gt          0.2192
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_restrained_S_all      0.923
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.739
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.138

#----------------------------------------------------------------------------#
#                   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 0 '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'
Cl Cl 0.1484 0.1585 '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 0.006 '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 0.3547(7) 0.4300(8) 0.6910(5) 0.0397(17) Uani 1 1 d . . . . .
C2 C 0.3687(7) 0.2978(8) 0.6913(5) 0.0430(18) Uani 1 1 d . . . . .
C3 C 0.3679(8) 0.1903(8) 0.7839(6) 0.0467(19) Uani 1 1 d . . . . .
C4 C 0.3537(8) 0.2156(10) 0.8736(6) 0.054(2) Uani 1 1 d . . . . .
H4 H 0.3546 0.1431 0.9351 0.065 Uiso 1 1 calc R U . . .
C5 C 0.3385(8) 0.3451(9) 0.8726(5) 0.0463(19) Uani 1 1 d . . . . .
H5 H 0.3276 0.3629 0.9333 0.056 Uiso 1 1 calc R U . . .
C6 C 0.3391(7) 0.4513(8) 0.7815(5) 0.0418(18) Uani 1 1 d . . . . .
C7 C 0.3454(7) 0.5141(8) 0.2370(6) 0.0431(18) Uani 1 1 d . . . . .
C8 C 0.3568(8) 0.4961(8) 0.1442(6) 0.0477(19) Uani 1 1 d . . . . .
C9 C 0.3541(9) 0.5997(10) 0.0566(6) 0.059(2) Uani 1 1 d . . . . .
H9 H 0.3664 0.5810 -0.0039 0.071 Uiso 1 1 calc R U . . .
C10 C 0.3331(9) 0.7373(10) 0.0532(6) 0.057(2) Uani 1 1 d . . . . .
H10 H 0.3279 0.8110 -0.0079 0.069 Uiso 1 1 calc R U . . .
C11 C 0.3212(8) 0.7559(9) 0.1418(6) 0.050(2) Uani 1 1 d . . . . .
C12 C 0.3255(7) 0.6500(8) 0.2352(5) 0.0386(17) Uani 1 1 d . . . . .
S1 S 0.36724(18) 0.56306(18) 0.57532(13) 0.0374(4) Uani 1 1 d . . . . .
S2 S 0.3822(2) 0.26951(19) 0.57836(14) 0.0411(5) Uani 1 1 d . . . . .
S3 S 0.3522(2) 0.3822(2) 0.35229(14) 0.0430(5) Uani 1 1 d . . . . .
S4 S 0.31792(19) 0.67633(19) 0.34951(13) 0.0405(4) Uani 1 1 d . . . . .
Cl1 Cl 0.3143(2) 0.6148(2) 0.78326(15) 0.0564(6) Uani 1 1 d . . . . .
Cl2 Cl 0.3885(2) 0.0247(2) 0.78971(16) 0.0605(6) Uani 1 1 d . . . . .
Cl3 Cl 0.3800(3) 0.3295(3) 0.14630(17) 0.0677(7) Uani 1 1 d . . . . .
Cl4 Cl 0.2969(2) 0.9230(2) 0.13874(17) 0.0602(6) Uani 1 1 d . . . . .
Fe1 Fe 0.39131(10) 0.46837(10) 0.45868(7) 0.0350(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.388(10) . ?
C1 C2 1.404(11) . ?
C1 S1 1.787(8) . ?
C2 C3 1.423(11) . ?
C2 S2 1.745(8) . ?
C3 C4 1.399(11) . ?
C3 Cl2 1.727(8) . ?
C4 C5 1.369(12) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(11) . ?
C5 H5 0.9500 . ?
C6 Cl1 1.737(8) . ?
C7 C8 1.405(10) . ?
C7 C12 1.428(11) . ?
C7 S3 1.757(8) . ?
C8 C9 1.354(12) . ?
C8 Cl3 1.752(9) . ?
C9 C10 1.437(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.348(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.419(11) . ?
C11 Cl4 1.752(9) . ?
C12 S4 1.760(7) . ?
S1 Fe1 2.225(2) . ?
S1 Fe1 2.494(2) 2_666 ?
S2 Fe1 2.244(2) . ?
S3 Fe1 2.194(2) . ?
S4 Fe1 2.244(2) . ?
Fe1 S1 2.494(2) 2_666 ?

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
C6 C1 C2 118.5(7) . . ?
C6 C1 S1 122.1(6) . . ?
C2 C1 S1 119.3(6) . . ?
C1 C2 C3 119.2(7) . . ?
C1 C2 S2 119.3(6) . . ?
C3 C2 S2 121.4(6) . . ?
C4 C3 C2 120.6(8) . . ?
C4 C3 Cl2 117.8(6) . . ?
C2 C3 Cl2 121.6(6) . . ?
C5 C4 C3 119.8(7) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.8(7) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C1 C6 C5 122.1(7) . . ?
C1 C6 Cl1 119.5(6) . . ?
C5 C6 Cl1 118.4(6) . . ?
C8 C7 C12 116.5(7) . . ?
C8 C7 S3 124.5(6) . . ?
C12 C7 S3 119.0(5) . . ?
C9 C8 C7 123.0(8) . . ?
C9 C8 Cl3 120.4(7) . . ?
C7 C8 Cl3 116.6(6) . . ?
C8 C9 C10 121.3(8) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C11 C10 C9 116.2(8) . . ?
C11 C10 H10 121.9 . . ?
C9 C10 H10 121.9 . . ?
C10 C11 C12 124.3(8) . . ?
C10 C11 Cl4 116.6(7) . . ?
C12 C11 Cl4 119.1(6) . . ?
C7 C12 C11 118.7(7) . . ?
C7 C12 S4 118.0(5) . . ?
C11 C12 S4 123.2(6) . . ?
C1 S1 Fe1 105.6(3) . . ?
C1 S1 Fe1 102.8(2) . 2_666 ?
Fe1 S1 Fe1 80.55(7) . 2_666 ?
C2 S2 Fe1 106.4(3) . . ?
C7 S3 Fe1 104.7(3) . . ?
C12 S4 Fe1 104.2(3) . . ?
S3 Fe1 S1 162.97(9) . . ?
S3 Fe1 S4 88.88(8) . . ?
S1 Fe1 S4 87.93(8) . . ?
S3 Fe1 S2 87.56(8) . . ?
S1 Fe1 S2 89.19(8) . . ?
S4 Fe1 S2 158.12(9) . . ?
S3 Fe1 S1 97.58(8) . 2_666 ?
S1 Fe1 S1 99.45(7) . 2_666 ?
S4 Fe1 S1 101.32(8) . 2_666 ?
S2 Fe1 S1 100.55(8) . 2_666 ?


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.005 -0.009 0.015 777 181 ' '
_platon_squeeze_details          
;The complex crystallized with four water molecules and one of acetone.
Due to the poor quality of the crystal, all of them presented severe
disorder and it was not posible to define a sensible chemical model, so 
Squeeze procedure was performed to remove their contribution to the structure
factors.
;
_database_code_depnum_ccdc_archive 'CCDC 1002771'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3

_audit_creation_date             2012-10-23T14:53:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

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

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C19 H4 Cl4 Fe3 O7 S4'
_chemical_formula_sum            'C19 H4 Cl4 Fe3 O7 S4'
_chemical_formula_weight         781.81
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration unk

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_Int_Tables_number      20
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   8.735(6)
_cell_length_b                   15.412(8)
_cell_length_c                   19.541(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2631(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    622
_cell_measurement_theta_min      3
_cell_measurement_theta_max      23
_cell_measurement_wavelength     0.71073

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

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.09
-11 -1 12 0.237
8 1 -1 0.299
0 0 1 0.083
-1 19 -2 0.035
1 -18 2 0.059

_exptl_special_details           
;
 ?
;

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

_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_T_max  0.664

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

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_ub_11      0.01
_diffrn_orient_matrix_ub_12      0
_diffrn_orient_matrix_ub_13      0
_diffrn_orient_matrix_ub_21      0
_diffrn_orient_matrix_ub_22      0.01
_diffrn_orient_matrix_ub_23      0
_diffrn_orient_matrix_ub_31      0
_diffrn_orient_matrix_ub_32      0
_diffrn_orient_matrix_ub_33      0.01
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_number            25690
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.37
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             3036
_reflns_number_gt                2476
_reflns_threshold_expression     >2σ(I)
_diffrn_reflns_reduction_process 
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;

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

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   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 > 2σ(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     
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3036
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0704
_refine_ls_wR_factor_gt          0.0654
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.877
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.520(17)
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.082

#----------------------------------------------------------------------------#
#                   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 0 '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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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 0.1567(5) 0.6315(3) 0.6145(2) 0.0284(11) Uani 1 1 d . . . . .
C2 C 0.2082(7) 0.7050(3) 0.6483(3) 0.0372(12) Uani 1 1 d . . . . .
C3 C 0.2567(7) 0.6999(3) 0.7158(3) 0.0453(14) Uani 1 1 d . . . . .
H3 H 0.2925 0.7493 0.7380 0.054 Uiso 1 1 calc R U . . .
C4 C 0.2516(8) 0.6215(3) 0.7502(3) 0.0456(15) Uani 1 1 d . . . . .
H4 H 0.2826 0.6183 0.7956 0.055 Uiso 1 1 calc R U . . .
C5 C 0.2008(6) 0.5482(3) 0.7170(2) 0.0325(11) Uani 1 1 d . . . . .
C6 C 0.1528(5) 0.5517(3) 0.6489(2) 0.0264(10) Uani 1 1 d . . . . .
C101 C -0.1535(7) 0.5000 0.5000 0.0287(14) Uani 1 2 d S T P . .
C201 C 0.4304(6) 0.5367(3) 0.4054(3) 0.0299(11) Uani 1 1 d . . . . .
C202 C 0.3043(6) 0.6923(3) 0.4126(2) 0.0312(10) Uani 1 1 d . . . . .
C203 C 0.4368(6) 0.6277(3) 0.5215(2) 0.0290(11) Uani 1 1 d . . . . .
Cl1 Cl 0.22332(18) 0.80320(7) 0.60517(7) 0.0465(4) Uani 1 1 d . . . . .
Cl2 Cl 0.2054(2) 0.44942(9) 0.75961(6) 0.0469(4) Uani 1 1 d . . . . .
Fe1 Fe 0.04533(9) 0.5000 0.5000 0.0216(2) Uani 1 2 d S T P . .
Fe2 Fe 0.29564(7) 0.59137(4) 0.46014(3) 0.02263(17) Uani 1 1 d . . . . .
O101 O -0.2845(6) 0.5000 0.5000 0.0560(14) Uani 1 2 d S T P . .
O201 O 0.5143(4) 0.5067(3) 0.3673(2) 0.0428(9) Uani 1 1 d . . . . .
O202 O 0.3120(5) 0.7551(2) 0.3824(2) 0.0460(10) Uani 1 1 d . . . . .
O203 O 0.5242(4) 0.6565(2) 0.55752(19) 0.0418(9) Uani 1 1 d . . . . .
S1 S 0.09452(13) 0.63596(7) 0.52793(6) 0.0245(3) Uani 1 1 d . . . . .
S2 S 0.09192(14) 0.45669(7) 0.60502(5) 0.0245(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.386(7) . ?
C1 C6 1.403(7) . ?
C1 S1 1.778(5) . ?
C2 C3 1.388(8) . ?
C2 Cl1 1.736(5) . ?
C3 C4 1.384(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(6) . ?
C5 Cl2 1.735(5) . ?
C6 S2 1.778(5) . ?
C101 O101 1.144(8) . ?
C101 Fe1 1.737(7) . ?
C201 O201 1.143(6) . ?
C201 Fe2 1.800(5) . ?
C202 O202 1.135(6) . ?
C202 Fe2 1.813(5) . ?
C203 O203 1.130(6) . ?
C203 Fe2 1.809(5) . ?
Fe1 S2 2.1960(14) 3_566 ?
Fe1 S2 2.1960(14) . ?
Fe1 S1 2.2076(15) 3_566 ?
Fe1 S1 2.2076(15) . ?
Fe1 Fe2 2.7149(16) . ?
Fe1 Fe2 2.7149(16) 3_566 ?
Fe2 S1 2.3052(16) . ?
Fe2 S2 2.3100(16) 3_566 ?
S2 Fe2 2.3100(16) 3_566 ?

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 C6 119.8(4) . . ?
C2 C1 S1 121.4(4) . . ?
C6 C1 S1 118.8(4) . . ?
C3 C2 C1 120.3(5) . . ?
C3 C2 Cl1 119.2(4) . . ?
C1 C2 Cl1 120.4(4) . . ?
C4 C3 C2 120.1(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.9(5) . . ?
C4 C5 Cl2 119.2(4) . . ?
C6 C5 Cl2 119.8(4) . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 S2 121.2(4) . . ?
C1 C6 S2 119.9(3) . . ?
O101 C101 Fe1 180.0 . . ?
O201 C201 Fe2 175.1(4) . . ?
O202 C202 Fe2 178.9(5) . . ?
O203 C203 Fe2 174.7(4) . . ?
C101 Fe1 S2 100.68(4) . 3_566 ?
C101 Fe1 S2 100.68(4) . . ?
S2 Fe1 S2 158.64(8) 3_566 . ?
C101 Fe1 S1 101.22(4) . 3_566 ?
S2 Fe1 S1 91.23(5) 3_566 3_566 ?
S2 Fe1 S1 84.63(5) . 3_566 ?
C101 Fe1 S1 101.22(4) . . ?
S2 Fe1 S1 84.63(5) 3_566 . ?
S2 Fe1 S1 91.23(5) . . ?
S1 Fe1 S1 157.55(7) 3_566 . ?
C101 Fe1 Fe2 143.65(3) . . ?
S2 Fe1 Fe2 54.90(4) 3_566 . ?
S2 Fe1 Fe2 106.05(5) . . ?
S1 Fe1 Fe2 105.35(5) 3_566 . ?
S1 Fe1 Fe2 54.68(4) . . ?
C101 Fe1 Fe2 143.65(3) . 3_566 ?
S2 Fe1 Fe2 106.05(5) 3_566 3_566 ?
S2 Fe1 Fe2 54.90(4) . 3_566 ?
S1 Fe1 Fe2 54.68(4) 3_566 3_566 ?
S1 Fe1 Fe2 105.35(5) . 3_566 ?
Fe2 Fe1 Fe2 72.71(5) . 3_566 ?
C201 Fe2 C203 95.3(2) . . ?
C201 Fe2 C202 94.0(2) . . ?
C203 Fe2 C202 92.6(2) . . ?
C201 Fe2 S1 168.39(15) . . ?
C203 Fe2 S1 92.66(16) . . ?
C202 Fe2 S1 94.05(16) . . ?
C201 Fe2 S2 91.50(16) . 3_566 ?
C203 Fe2 S2 171.80(15) . 3_566 ?
C202 Fe2 S2 91.40(16) . 3_566 ?
S1 Fe2 S2 79.93(6) . 3_566 ?
C201 Fe2 Fe1 117.04(15) . . ?
C203 Fe2 Fe1 121.30(15) . . ?
C202 Fe2 Fe1 128.71(16) . . ?
S1 Fe2 Fe1 51.39(4) . . ?
S2 Fe2 Fe1 51.05(4) 3_566 . ?
C1 S1 Fe1 104.96(16) . . ?
C1 S1 Fe2 107.61(16) . . ?
Fe1 S1 Fe2 73.93(5) . . ?
C6 S2 Fe1 104.84(15) . . ?
C6 S2 Fe2 107.42(16) . 3_566 ?
Fe1 S2 Fe2 74.05(5) . 3_566 ?

# END of CIF



_database_code_depnum_ccdc_archive 'CCDC 1002772'
