# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 972917'
_audit_update_record             
;
2013-11-20 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H8 Cl2 Fe O4 S8'
_chemical_formula_weight         599.41

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'
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'
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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.896(2)
_cell_length_b                   11.401(3)
_cell_length_c                   11.427(3)
_cell_angle_alpha                112.062(2)
_cell_angle_beta                 103.775(2)
_cell_angle_gamma                100.328(4)
_cell_volume                     995.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    3589
_cell_measurement_theta_min      2.0196
_cell_measurement_theta_max      27.4757

_exptl_crystal_description       rod
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_absorpt_coefficient_mu    1.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7888
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17763
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4554
_reflns_number_gt                4300
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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     
'calc w=1/[σ²(Fo²)+(0.0305P)²+1.0321P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4554
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0796
_refine_ls_wR_factor_gt          0.0780
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.67710(4) 0.37559(3) 0.35496(3) 0.01640(9) Uani 1 1 d . . .
Cl1 Cl 0.70967(8) 0.17183(6) 0.30202(6) 0.02278(14) Uani 1 1 d . . .
Cl2 Cl 0.52208(8) 0.33783(7) 0.14945(6) 0.02646(15) Uani 1 1 d . . .
S1 S 0.65499(7) 0.05410(6) -0.07901(6) 0.01806(13) Uani 1 1 d . . .
S2 S 0.94174(7) 0.28455(6) 0.05165(6) 0.02089(14) Uani 1 1 d . . .
S3 S 0.82414(7) -0.08056(6) 0.09120(6) 0.01798(13) Uani 1 1 d . . .
S4 S 1.11107(7) 0.15200(6) 0.23224(6) 0.01942(13) Uani 1 1 d . . .
S5 S 0.46053(7) 0.16059(6) -0.23916(6) 0.02022(14) Uani 1 1 d . . .
S6 S 0.80816(10) 0.43535(8) -0.08441(10) 0.0504(3) Uani 1 1 d . . .
S7 S 0.92662(8) -0.21915(7) 0.24955(7) 0.02763(16) Uani 1 1 d . . .
S8 S 1.27315(8) 0.06309(7) 0.42669(7) 0.02529(15) Uani 1 1 d . . .
O1 O 0.6478(2) 0.56649(17) 0.44758(17) 0.0189(3) Uani 1 1 d . . .
O2 O 0.8465(2) 0.44092(17) 0.55190(17) 0.0194(4) Uani 1 1 d . . .
O3 O 0.8850(2) 0.46779(18) 0.33897(17) 0.0205(4) Uani 1 1 d . . .
O4 O 0.4965(2) 0.33498(17) 0.43022(17) 0.0203(4) Uani 1 1 d . . .
C1 C 0.8491(3) 0.1301(2) 0.0332(2) 0.0159(5) Uani 1 1 d . . .
C2 C 0.9240(3) 0.0718(2) 0.1080(2) 0.0162(5) Uani 1 1 d . . .
C3 C 0.6447(3) 0.1828(2) -0.1244(2) 0.0176(5) Uani 1 1 d . . .
C4 C 0.7796(3) 0.2898(3) -0.0644(3) 0.0219(5) Uani 1 1 d . . .
C5 C 0.9712(3) -0.0764(2) 0.2251(2) 0.0182(5) Uani 1 1 d . . .
C6 C 1.1042(3) 0.0308(2) 0.2913(2) 0.0191(5) Uani 1 1 d . . .
C7 C 0.4798(3) 0.3294(3) -0.2164(3) 0.0244(5) Uani 1 1 d . . .
H7A H 0.3872 0.3291 -0.2848 0.029 Uiso 1 1 calc R . .
H7B H 0.4738 0.3822 -0.1272 0.029 Uiso 1 1 calc R . .
C8 C 0.6357(3) 0.3956(3) -0.2268(3) 0.0241(5) Uani 1 1 d . . .
H8A H 0.6275 0.4779 -0.2348 0.029 Uiso 1 1 calc R . .
H8B H 0.6513 0.3359 -0.3090 0.029 Uiso 1 1 calc R . .
C9 C 1.0761(3) -0.1664(3) 0.4114(3) 0.0253(6) Uani 1 1 d . . .
H9A H 1.0441 -0.1037 0.4812 0.030 Uiso 1 1 calc R . .
H9B H 1.0780 -0.2445 0.4298 0.030 Uiso 1 1 calc R . .
C10 C 1.2453(3) -0.0999(3) 0.4207(3) 0.0223(5) Uani 1 1 d . . .
H10A H 1.2697 -0.1571 0.3423 0.027 Uiso 1 1 calc R . .
H10B H 1.3244 -0.0930 0.5021 0.027 Uiso 1 1 calc R . .
C11 C 0.5443(3) 0.5673(2) 0.5051(2) 0.0162(5) Uani 1 1 d . . .
C12 C 0.9885(3) 0.4926(2) 0.5619(2) 0.0161(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O3 2.0418(18) . ?
Fe1 O4 2.0558(18) . ?
Fe1 O1 2.1281(18) . ?
Fe1 O2 2.1479(18) . ?
Fe1 Cl2 2.2556(9) . ?
Fe1 Cl1 2.2618(9) . ?
S1 C1 1.718(2) . ?
S1 C3 1.740(2) . ?
S2 C1 1.715(2) . ?
S2 C4 1.739(2) . ?
S3 C2 1.720(2) . ?
S3 C5 1.739(2) . ?
S4 C2 1.724(2) . ?
S4 C6 1.749(2) . ?
S5 C3 1.745(2) . ?
S5 C7 1.813(3) . ?
S6 C4 1.741(3) . ?
S6 C8 1.793(3) . ?
S7 C5 1.746(2) . ?
S7 C9 1.805(3) . ?
S8 C6 1.747(2) . ?
S8 C10 1.803(3) . ?
O1 C11 1.252(3) . ?
O2 C12 1.253(3) . ?
O3 C12 1.256(3) 2_766 ?
O4 C11 1.254(3) 2_666 ?
C1 C2 1.390(3) . ?
C3 C4 1.362(3) . ?
C5 C6 1.352(3) . ?
C7 C8 1.509(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.518(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 O4 1.254(3) 2_666 ?
C11 C11 1.542(4) 2_666 ?
C12 O3 1.256(3) 2_766 ?
C12 C12 1.542(4) 2_766 ?

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
O3 Fe1 O4 161.48(7) . . ?
O3 Fe1 O1 87.44(7) . . ?
O4 Fe1 O1 78.59(7) . . ?
O3 Fe1 O2 78.62(7) . . ?
O4 Fe1 O2 87.25(7) . . ?
O1 Fe1 O2 81.43(7) . . ?
O3 Fe1 Cl2 93.73(5) . . ?
O4 Fe1 Cl2 99.04(6) . . ?
O1 Fe1 Cl2 93.01(5) . . ?
O2 Fe1 Cl2 170.68(5) . . ?
O3 Fe1 Cl1 98.98(6) . . ?
O4 Fe1 Cl1 92.48(5) . . ?
O1 Fe1 Cl1 166.78(5) . . ?
O2 Fe1 Cl1 88.49(5) . . ?
Cl2 Fe1 Cl1 98.05(3) . . ?
C1 S1 C3 95.54(11) . . ?
C1 S2 C4 95.55(12) . . ?
C2 S3 C5 95.00(11) . . ?
C2 S4 C6 95.21(12) . . ?
C3 S5 C7 100.77(12) . . ?
C4 S6 C8 102.90(12) . . ?
C5 S7 C9 100.89(12) . . ?
C6 S8 C10 100.23(12) . . ?
C11 O1 Fe1 113.15(15) . . ?
C12 O2 Fe1 112.37(15) . . ?
C12 O3 Fe1 115.90(15) 2_766 . ?
C11 O4 Fe1 115.72(15) 2_666 . ?
C2 C1 S2 122.12(18) . . ?
C2 C1 S1 121.85(18) . . ?
S2 C1 S1 115.99(13) . . ?
C1 C2 S3 120.71(18) . . ?
C1 C2 S4 122.86(19) . . ?
S3 C2 S4 116.16(13) . . ?
C4 C3 S1 116.33(18) . . ?
C4 C3 S5 127.71(19) . . ?
S1 C3 S5 115.94(14) . . ?
C3 C4 S2 116.57(19) . . ?
C3 C4 S6 128.05(19) . . ?
S2 C4 S6 115.34(15) . . ?
C6 C5 S3 117.48(18) . . ?
C6 C5 S7 129.09(19) . . ?
S3 C5 S7 113.37(14) . . ?
C5 C6 S8 128.49(19) . . ?
C5 C6 S4 116.09(18) . . ?
S8 C6 S4 115.41(14) . . ?
C8 C7 S5 113.45(18) . . ?
C8 C7 H7A 108.9 . . ?
S5 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
S5 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 S6 112.16(18) . . ?
C7 C8 H8A 109.2 . . ?
S6 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
S6 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C10 C9 S7 112.84(18) . . ?
C10 C9 H9A 109.0 . . ?
S7 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
S7 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 S8 114.37(18) . . ?
C9 C10 H10A 108.7 . . ?
S8 C10 H10A 108.7 . . ?
C9 C10 H10B 108.7 . . ?
S8 C10 H10B 108.7 . . ?
H10A C10 H10B 107.6 . . ?
O1 C11 O4 127.5(2) . 2_666 ?
O1 C11 C11 116.4(3) . 2_666 ?
O4 C11 C11 116.1(3) 2_666 2_666 ?
O2 C12 O3 127.3(2) . 2_766 ?
O2 C12 C12 116.5(3) . 2_766 ?
O3 C12 C12 116.2(3) 2_766 2_766 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C7 H7A O1 0.99 2.55 3.330(3) 135.7 2_665
C10 H10A S5 0.99 2.91 3.713(3) 138.4 2_755
C8 H8A Cl2 0.99 2.69 3.477(3) 137.1 2_665
C10 H10B Cl1 0.99 2.77 3.513(3) 132.7 2_756
C9 H9B O2 0.99 2.52 3.474(3) 162.3 2_756
C9 H9B Cl1 0.99 2.90 3.403(3) 112.3 2_756

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.089
