# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# 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_feesa_compound_1
_database_code_depnum_ccdc_archive 'CCDC 1037915'
_audit_update_record             
;
2014-12-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H30 Fe N6 S6 2+, 2(B F4 1-)'
_chemical_formula_sum            'C18 H30 B2 F8 Fe N6 S6'
_chemical_formula_weight         752.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c
_symmetry_space_group_name_Hall  '-C 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   22.662(5)
_cell_length_b                   11.130(3)
_cell_length_c                   18.004(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 134.54(2)
_cell_angle_gamma                90.00
_cell_volume                     3236.7(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24
_cell_measurement_theta_min      6.12
_cell_measurement_theta_max      16.81

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
local program based on Walker & Stuart,
(a) Walker, N.; Stuart, D. Acta Crystallogr., Sect. A 1983, 39, 158;
(b) Ugozzoli, F. Comput. Chem. 1987, 11, 109
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Philips PW 1100 diffractometer'
_diffrn_measurement_method       theta-2-theta
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3258
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_sigmaI/netI    0.1571
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3160
_reflns_number_gt                1188
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'local program'
_computing_cell_refinement       'local program'
_computing_data_reduction        'local program'
_computing_structure_solution    Sir97
_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.
 The BF4- was found disordered in three positions that were each refined with
 site occupancy factors (s.o.f.) of 0.33. The three fraction of the BF4- were
 refined isotropically.
 The complex lies on a binary axis and one of the ligands was disordered in
 two positions with s.o.f. of 0.5.
 
;

_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)+(0.0001P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         3160
_refine_ls_number_parameters     189
_refine_ls_number_restraints     32
_refine_ls_R_factor_all          0.1700
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.0711
_refine_ls_wR_factor_gt          0.0592
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      1.049
_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
Fe Fe 0.5000 0.00196(14) 0.2500 0.0376(3) Uani 1 2 d S . .
S13 S 0.59476(11) 0.14862(16) 0.35761(13) 0.0447(5) Uani 1 1 d . A .
S21 S 0.56129(8) -0.01147(19) 0.18823(10) 0.0455(4) Uani 1 1 d . . .
S11 S 0.40182(11) -0.13504(16) 0.12803(13) 0.0467(5) Uani 1 1 d . . .
C31 C 0.4868(5) -0.2547(6) -0.0266(5) 0.073(2) Uani 1 1 d . . .
H31A H 0.5076 -0.3322 0.0078 0.088 Uiso 1 1 calc R . .
H31B H 0.4949 -0.2484 -0.0726 0.088 Uiso 1 1 calc R . .
N21 N 0.3760(3) -0.2356(4) -0.0244(4) 0.0518(15) Uani 1 1 d . . .
C11 C 0.4265(3) -0.1657(5) 0.0599(4) 0.0417(16) Uani 1 1 d . . .
N11 N 0.5326(3) -0.1587(4) 0.0516(4) 0.0539(15) Uani 1 1 d . . .
C61 C 0.2951(3) -0.2863(5) -0.0638(4) 0.070(2) Uani 1 1 d . . .
H61A H 0.3058 -0.3213 -0.0066 0.106 Uiso 1 1 calc R . .
H61B H 0.2736 -0.3466 -0.1156 0.106 Uiso 1 1 calc R . .
H61C H 0.2554 -0.2227 -0.0937 0.106 Uiso 1 1 calc R . .
C13 C 0.5453(3) 0.2807(5) 0.3014(4) 0.0579(15) Uani 1 1 d . . .
N23 N 0.5814(9) 0.3816(13) 0.3620(11) 0.0579(15) Uani 0.50 1 d PD A -1
N13 N 0.4141(9) 0.3861(13) 0.1649(10) 0.0579(15) Uani 0.50 1 d PD . -1
C33 C 0.4598(7) 0.5020(13) 0.2122(9) 0.0579(15) Uani 0.50 1 d P A -1
H33A H 0.4785 0.5272 0.1800 0.070 Uiso 0.50 1 calc PR A -1
H33B H 0.4223 0.5631 0.1978 0.070 Uiso 0.50 1 calc PR A -1
C43 C 0.5319(8) 0.4932(14) 0.3260(9) 0.0579(15) Uani 0.50 1 d P A -1
H43A H 0.5125 0.4988 0.3597 0.070 Uiso 0.50 1 calc PR A -1
H43B H 0.5678 0.5615 0.3488 0.070 Uiso 0.50 1 calc PR A -1
C53 C 0.3214(7) 0.3962(11) 0.0682(9) 0.0579(15) Uani 0.50 1 d PD B -1
H53A H 0.2946 0.4318 0.0868 0.087 Uiso 0.50 1 calc PR B -1
H53B H 0.2988 0.3177 0.0396 0.087 Uiso 0.50 1 calc PR B -1
H53C H 0.3123 0.4456 0.0172 0.087 Uiso 0.50 1 calc PR B -1
C63 C 0.6671(7) 0.3835(11) 0.4669(9) 0.0579(15) Uani 0.50 1 d PD A -1
H63A H 0.6658 0.3915 0.5188 0.087 Uiso 0.50 1 calc PR A -1
H63C H 0.6966 0.4502 0.4718 0.087 Uiso 0.50 1 calc PR A -1
H63B H 0.6946 0.3100 0.4781 0.087 Uiso 0.50 1 calc PR A -1
C21 C 0.5058(4) -0.1171(5) 0.0948(4) 0.0415(16) Uani 1 1 d . . .
C41 C 0.3904(4) -0.2450(6) -0.0929(5) 0.071(2) Uani 1 1 d . . .
H41A H 0.3675 -0.1749 -0.1377 0.085 Uiso 1 1 calc R . .
H41B H 0.3621 -0.3154 -0.1370 0.085 Uiso 1 1 calc R . .
C51 C 0.6185(4) -0.1297(6) 0.0937(5) 0.074(2) Uani 1 1 d . . .
H51A H 0.6184 -0.0491 0.0745 0.112 Uiso 1 1 calc R . .
H51B H 0.6301 -0.1849 0.0644 0.112 Uiso 1 1 calc R . .
H51C H 0.6602 -0.1370 0.1682 0.112 Uiso 1 1 calc R . .
B B 0.6574(7) 0.5454(10) 0.2203(9) 0.127(5) Uiso 1 1 d D . .
F1A F 0.6250(10) 0.6580(11) 0.2062(12) 0.081(7) Uiso 0.33 1 d PD C 1
F2A F 0.7188(8) 0.5233(15) 0.3370(10) 0.118(6) Uiso 0.33 1 d PD C 1
F3A F 0.5971(9) 0.4463(11) 0.2001(13) 0.095(5) Uiso 0.33 1 d PD C 1
F4A F 0.6825(11) 0.5320(18) 0.1783(14) 0.134(7) Uiso 0.33 1 d PD C 1
F1B F 0.6079(10) 0.6401(14) 0.2133(15) 0.057(5) Uiso 0.33 1 d PD C 2
F2B F 0.6615(12) 0.4461(12) 0.2614(13) 0.107(5) Uiso 0.33 1 d PD C 2
F3B F 0.6161(7) 0.5261(11) 0.1080(8) 0.077(4) Uiso 0.33 1 d PD C 2
F4B F 0.7329(10) 0.583(2) 0.2598(18) 0.181(10) Uiso 0.33 1 d PD C 2
F1C F 0.7155(12) 0.483(2) 0.2988(15) 0.163(9) Uiso 0.33 1 d PD C 3
F2C F 0.5788(9) 0.497(2) 0.1366(13) 0.181(7) Uiso 0.33 1 d PD C 3
F3C F 0.7003(14) 0.6061(19) 0.199(2) 0.175(11) Uiso 0.33 1 d PD C 3
F4C F 0.6236(14) 0.6264(18) 0.2493(17) 0.168(13) Uiso 0.33 1 d PD C 3


_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
Fe S13 2.279(2) . ?
Fe S13 2.279(2) 2_655 ?
Fe S11 2.290(2) . ?
Fe S11 2.290(2) 2_655 ?
Fe S21 2.3141(14) 2_655 ?
Fe S21 2.3141(14) . ?
S13 C13 1.689(5) . ?
S21 C21 1.681(6) . ?
S11 C11 1.701(6) . ?
C31 N11 1.467(6) . ?
C31 C41 1.596(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
N21 C11 1.334(6) . ?
N21 C41 1.485(7) . ?
N21 C61 1.536(6) . ?
C11 C21 1.529(7) . ?
N11 C21 1.360(6) . ?
N11 C51 1.548(7) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C13 N13 1.344(14) 2_655 ?
C13 N23 1.367(14) . ?
C13 C13 1.519(10) 2_655 ?
N23 C63 1.482(12) . ?
N23 C43 1.483(18) . ?
N13 C13 1.344(14) 2_655 ?
N13 C33 1.492(18) . ?
N13 C53 1.526(12) . ?
C33 C43 1.477(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63C 0.9600 . ?
C63 H63B 0.9600 . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
B F4A 1.235(13) . ?
B F1C 1.268(15) . ?
B F2B 1.297(13) . ?
B F4B 1.381(15) . ?
B F1A 1.382(14) . ?
B F2C 1.401(14) . ?
B F3C 1.439(15) . ?
B F1B 1.478(14) . ?
B F4C 1.494(16) . ?
B F2A 1.519(14) . ?
B F3B 1.535(13) . ?
B F3A 1.586(13) . ?

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
S13 Fe S13 88.50(10) . 2_655 ?
S13 Fe S11 174.05(8) . . ?
S13 Fe S11 87.67(6) 2_655 . ?
S13 Fe S11 87.67(6) . 2_655 ?
S13 Fe S11 174.05(8) 2_655 2_655 ?
S11 Fe S11 96.50(11) . 2_655 ?
S13 Fe S21 99.38(7) . 2_655 ?
S13 Fe S21 85.96(7) 2_655 2_655 ?
S11 Fe S21 84.89(7) . 2_655 ?
S11 Fe S21 90.18(7) 2_655 2_655 ?
S13 Fe S21 85.96(7) . . ?
S13 Fe S21 99.38(7) 2_655 . ?
S11 Fe S21 90.18(7) . . ?
S11 Fe S21 84.89(7) 2_655 . ?
S21 Fe S21 172.59(13) 2_655 . ?
C13 S13 Fe 106.3(2) . . ?
C21 S21 Fe 104.3(2) . . ?
C11 S11 Fe 103.6(2) . . ?
N11 C31 C41 110.2(5) . . ?
N11 C31 H31A 109.6 . . ?
C41 C31 H31A 109.6 . . ?
N11 C31 H31B 109.6 . . ?
C41 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
C11 N21 C41 118.3(5) . . ?
C11 N21 C61 122.2(5) . . ?
C41 N21 C61 118.5(5) . . ?
N21 C11 C21 119.8(5) . . ?
N21 C11 S11 119.0(5) . . ?
C21 C11 S11 121.3(4) . . ?
C21 N11 C31 119.8(5) . . ?
C21 N11 C51 124.2(5) . . ?
C31 N11 C51 115.0(5) . . ?
N21 C61 H61A 109.5 . . ?
N21 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N21 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N13 C13 N23 23.9(9) 2_655 . ?
N13 C13 C13 117.5(7) 2_655 2_655 ?
N23 C13 C13 120.9(7) . 2_655 ?
N13 C13 S13 122.2(7) 2_655 . ?
N23 C13 S13 117.6(7) . . ?
C13 C13 S13 119.46(18) 2_655 . ?
C13 N23 C63 123.0(12) . . ?
C13 N23 C43 119.6(10) . . ?
C63 N23 C43 117.3(11) . . ?
C13 N13 C33 121.1(11) 2_655 . ?
C13 N13 C53 122.6(12) 2_655 . ?
C33 N13 C53 115.8(11) . . ?
C43 C33 N13 112.6(15) . . ?
C43 C33 H33A 109.1 . . ?
N13 C33 H33A 109.1 . . ?
C43 C33 H33B 109.1 . . ?
N13 C33 H33B 109.1 . . ?
H33A C33 H33B 107.8 . . ?
C33 C43 N23 115.0(13) . . ?
C33 C43 H43A 108.5 . . ?
N23 C43 H43A 108.5 . . ?
C33 C43 H43B 108.5 . . ?
N23 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
N11 C21 C11 120.8(5) . . ?
N11 C21 S21 119.3(5) . . ?
C11 C21 S21 119.8(4) . . ?
N21 C41 C31 111.4(5) . . ?
N21 C41 H41A 109.3 . . ?
C31 C41 H41A 109.3 . . ?
N21 C41 H41B 109.3 . . ?
C31 C41 H41B 109.3 . . ?
H41A C41 H41B 108.0 . . ?
N11 C51 H51A 109.5 . . ?
N11 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N11 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
F4A B F1C 92.9(15) . . ?
F4A B F2B 111.5(15) . . ?
F1C B F2B 44.9(11) . . ?
F4A B F4B 54.0(12) . . ?
F1C B F4B 69.4(13) . . ?
F2B B F4B 113.4(15) . . ?
F4A B F1A 114.2(14) . . ?
F1C B F1A 135.0(16) . . ?
F2B B F1A 134.0(13) . . ?
F4B B F1A 97.3(14) . . ?
F4A B F2C 94.6(13) . . ?
F1C B F2C 122.1(16) . . ?
F2B B F2C 79.5(12) . . ?
F4B B F2C 148.3(15) . . ?
F1A B F2C 92.2(13) . . ?
F4A B F3C 37.4(12) . . ?
F1C B F3C 100.7(15) . . ?
F2B B F3C 139.4(15) . . ?
F4B B F3C 33.8(12) . . ?
F1A B F3C 84.0(12) . . ?
F2C B F3C 118.6(16) . . ?
F4A B F1B 133.0(16) . . ?
F1C B F1B 128.4(16) . . ?
F2B B F1B 113.8(14) . . ?
F4B B F1B 114.9(14) . . ?
F1A B F1B 20.8(10) . . ?
F2C B F1B 82.2(12) . . ?
F3C B F1B 104.8(15) . . ?
F4A B F4C 149.0(16) . . ?
F1C B F4C 109.3(15) . . ?
F2B B F4C 99.5(13) . . ?
F4B B F4C 113.1(15) . . ?
F1A B F4C 35.1(10) . . ?
F2C B F4C 91.7(13) . . ?
F3C B F4C 114.7(15) . . ?
F1B B F4C 19.2(12) . . ?
F4A B F2A 117.3(14) . . ?
F1C B F2A 30.9(12) . . ?
F2B B F2A 56.2(11) . . ?
F4B B F2A 74.6(13) . . ?
F1A B F2A 104.8(12) . . ?
F2C B F2A 131.8(14) . . ?
F3C B F2A 108.0(14) . . ?
F1B B F2A 97.9(12) . . ?
F4C B F2A 79.1(11) . . ?
F4A B F3B 45.0(9) . . ?
F1C B F3B 125.9(15) . . ?
F2B B F3B 111.4(11) . . ?
F4B B F3B 96.3(12) . . ?
F1A B F3B 97.5(11) . . ?
F2C B F3B 52.4(9) . . ?
F3C B F3B 67.5(12) . . ?
F1B B F3B 105.2(11) . . ?
F4C B F3B 123.8(13) . . ?
F2A B F3B 156.8(12) . . ?
F4A B F3A 118.0(14) . . ?
F1C B F3A 85.8(13) . . ?
F2B B F3A 40.9(8) . . ?
F4B B F3A 152.4(14) . . ?
F1A B F3A 109.1(11) . . ?
F2C B F3A 41.3(9) . . ?
F3C B F3A 154.1(15) . . ?
F1B B F3A 89.8(11) . . ?
F4C B F3A 86.0(11) . . ?
F2A B F3A 90.6(10) . . ?
F3B B F3A 88.3(10) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_fesa_compound-2
_database_code_depnum_ccdc_archive 'CCDC 1037916'
_audit_update_record             
;
2014-12-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H20 Cl2 Fe N4 O2 S2 1+, B F4 1-'
_chemical_formula_sum            'C12 H20 B Cl2 F4 Fe N4 O2 S2'
_chemical_formula_weight         530.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
Cl Cl 0.1484 0.1585 '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'
B B 0.0013 0.0007 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.978(1)
_cell_length_b                   12.495(1)
_cell_length_c                   17.672(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.174(5)
_cell_angle_gamma                90.00
_cell_volume                     2186.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11886
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1076
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart 1000 area detector'
_diffrn_measurement_method       theta-2-theta
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            23266
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.51
_reflns_number_total             4893
_reflns_number_gt                3647
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for windows'
_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.
 The BF4- anion was found disordered in two positions with s.o.f. of
 0.63/0.37
 
;

_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)+(0.0525P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         4893
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0860
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_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
C11 C -0.0370(2) 0.25289(17) 0.01179(13) 0.0413(5) Uani 1 1 d . . .
C21 C 0.0092(2) 0.14635(16) 0.04598(12) 0.0379(4) Uani 1 1 d . . .
C31 C -0.2198(2) 0.1201(2) 0.07478(17) 0.0601(7) Uani 1 1 d . . .
H31B H -0.2327 0.1627 0.1192 0.072 Uiso 1 1 calc R . .
H31A H -0.2754 0.0565 0.0752 0.072 Uiso 1 1 calc R . .
C41 C -0.2629(2) 0.1826(2) 0.00494(19) 0.0680(8) Uani 1 1 d . . .
H41A H -0.2681 0.1359 -0.0392 0.082 Uiso 1 1 calc R . .
H41B H -0.3521 0.2121 0.0076 0.082 Uiso 1 1 calc R . .
C51 C -0.0329(3) -0.0024(2) 0.12730(15) 0.0589(6) Uani 1 1 d . . .
H51A H 0.0639 -0.0070 0.1326 0.088 Uiso 1 1 calc R . .
H51C H -0.0712 -0.0670 0.1045 0.088 Uiso 1 1 calc R . .
H51B H -0.0619 0.0068 0.1767 0.088 Uiso 1 1 calc R . .
C61 C -0.2206(3) 0.3729(2) -0.0345(2) 0.0863(10) Uani 1 1 d . . .
H61B H -0.2912 0.3965 -0.0063 0.129 Uiso 1 1 calc R . .
H61A H -0.2562 0.3640 -0.0872 0.129 Uiso 1 1 calc R . .
H61C H -0.1495 0.4251 -0.0303 0.129 Uiso 1 1 calc R . .
C12 C 0.4037(2) 0.10462(16) 0.19197(12) 0.0394(5) Uani 1 1 d . . .
C22 C 0.2916(2) 0.18136(17) 0.20388(12) 0.0404(5) Uani 1 1 d . . .
C32 C 0.2747(3) 0.0898(2) 0.32220(14) 0.0589(7) Uani 1 1 d . . .
H32A H 0.2291 0.0227 0.3085 0.071 Uiso 1 1 calc R . .
H32B H 0.2512 0.1119 0.3715 0.071 Uiso 1 1 calc R . .
C42 C 0.4232(3) 0.0746(2) 0.32693(13) 0.0608(7) Uani 1 1 d . . .
H42B H 0.4689 0.1384 0.3481 0.073 Uiso 1 1 calc R . .
H42A H 0.4506 0.0151 0.3606 0.073 Uiso 1 1 calc R . .
C52 C 0.1080(3) 0.2317(3) 0.27285(16) 0.0707(8) Uani 1 1 d . . .
H52B H 0.1295 0.3065 0.2773 0.106 Uiso 1 1 calc R . .
H52C H 0.0709 0.2083 0.3176 0.106 Uiso 1 1 calc R . .
H52A H 0.0432 0.2202 0.2287 0.106 Uiso 1 1 calc R . .
C62 C 0.5756(3) -0.0203(2) 0.24508(17) 0.0633(7) Uani 1 1 d . . .
H62A H 0.5532 -0.0672 0.2023 0.095 Uiso 1 1 calc R . .
H62C H 0.5922 -0.0620 0.2910 0.095 Uiso 1 1 calc R . .
H62B H 0.6550 0.0200 0.2382 0.095 Uiso 1 1 calc R . .
F4 F 0.1791(7) 0.8270(6) 0.1760(4) 0.168(3) Uani 0.63 1 d P A 1
F2 F 0.2484(15) 0.8232(6) 0.3011(4) 0.181(5) Uani 0.63 1 d P A 1
F3 F 0.3814(6) 0.7673(6) 0.2123(5) 0.159(3) Uani 0.63 1 d P A 1
F1 F 0.2075(6) 0.6781(5) 0.2390(4) 0.0994(16) Uani 0.63 1 d P A 1
N11 N -0.07760(18) 0.08877(14) 0.07891(11) 0.0443(4) Uani 1 1 d . . .
N21 N -0.16685(19) 0.27018(15) -0.00364(13) 0.0542(5) Uani 1 1 d . . .
N12 N 0.2308(2) 0.17085(15) 0.26508(10) 0.0477(5) Uani 1 1 d . . .
N22 N 0.46286(19) 0.05319(15) 0.25095(10) 0.0460(4) Uani 1 1 d . . .
B B 0.2583(5) 0.7846(4) 0.2322(3) 0.0864(11) Uani 1 1 d . . .
S11 S 0.08465(6) 0.34135(4) -0.00037(4) 0.04899(16) Uani 1 1 d . . .
S12 S 0.44055(6) 0.09074(5) 0.10232(3) 0.04785(15) Uani 1 1 d . . .
Fe Fe 0.28770(3) 0.22826(2) 0.040717(16) 0.03705(10) Uani 1 1 d . . .
Cl1 Cl 0.33799(6) 0.16399(5) -0.07252(3) 0.05318(16) Uani 1 1 d . . .
Cl2 Cl 0.41574(6) 0.37713(5) 0.03881(4) 0.05503(16) Uani 1 1 d . . .
O21 O 0.12937(14) 0.11868(11) 0.04568(9) 0.0455(4) Uani 1 1 d . . .
O22 O 0.25578(16) 0.24998(12) 0.15326(8) 0.0489(4) Uani 1 1 d . . .
F5 F 0.3837(14) 0.7891(10) 0.2681(9) 0.171(7) Uani 0.37 1 d P A 2
F7 F 0.2634(11) 0.8730(9) 0.1842(7) 0.157(4) Uani 0.37 1 d P A 2
F8 F 0.1761(15) 0.8439(12) 0.2729(14) 0.210(11) Uani 0.37 1 d P A 2
F6 F 0.209(2) 0.7053(13) 0.2077(11) 0.223(10) Uani 0.37 1 d P A 2


_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
C11 N21 1.308(3) . ?
C11 C21 1.510(3) . ?
C11 S11 1.675(2) . ?
C21 O21 1.248(2) . ?
C21 N11 1.316(3) . ?
C31 N11 1.465(3) . ?
C31 C41 1.478(4) . ?
C31 H31B 0.9700 . ?
C31 H31A 0.9700 . ?
C41 N21 1.475(3) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C51 N11 1.461(3) . ?
C51 H51A 0.9600 . ?
C51 H51C 0.9600 . ?
C51 H51B 0.9600 . ?
C61 N21 1.469(3) . ?
C61 H61B 0.9600 . ?
C61 H61A 0.9600 . ?
C61 H61C 0.9600 . ?
C12 N22 1.301(3) . ?
C12 C22 1.508(3) . ?
C12 S12 1.679(2) . ?
C22 O22 1.258(2) . ?
C22 N12 1.311(3) . ?
C32 N12 1.458(3) . ?
C32 C42 1.486(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C42 N22 1.471(3) . ?
C42 H42B 0.9700 . ?
C42 H42A 0.9700 . ?
C52 N12 1.462(3) . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C52 H52A 0.9600 . ?
C62 N22 1.466(3) . ?
C62 H62A 0.9600 . ?
C62 H62C 0.9600 . ?
C62 H62B 0.9600 . ?
F4 B 1.301(7) . ?
F2 B 1.325(9) . ?
F3 B 1.337(7) . ?
F1 B 1.434(8) . ?
B F6 1.165(17) . ?
B F5 1.333(11) . ?
B F8 1.374(15) . ?
B F7 1.397(10) . ?
S11 Fe 2.5022(7) . ?
S12 Fe 2.4595(6) . ?
Fe O22 2.0709(15) . ?
Fe O21 2.1007(14) . ?
Fe Cl2 2.2592(6) . ?
Fe Cl1 2.2699(7) . ?

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
N21 C11 C21 118.32(19) . . ?
N21 C11 S11 125.38(17) . . ?
C21 C11 S11 116.27(15) . . ?
O21 C21 N11 122.41(19) . . ?
O21 C21 C11 119.22(18) . . ?
N11 C21 C11 118.25(18) . . ?
N11 C31 C41 111.2(2) . . ?
N11 C31 H31B 109.4 . . ?
C41 C31 H31B 109.4 . . ?
N11 C31 H31A 109.4 . . ?
C41 C31 H31A 109.4 . . ?
H31B C31 H31A 108.0 . . ?
N21 C41 C31 110.7(2) . . ?
N21 C41 H41A 109.5 . . ?
C31 C41 H41A 109.5 . . ?
N21 C41 H41B 109.5 . . ?
C31 C41 H41B 109.5 . . ?
H41A C41 H41B 108.1 . . ?
N11 C51 H51A 109.5 . . ?
N11 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
N11 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51C C51 H51B 109.5 . . ?
N21 C61 H61B 109.5 . . ?
N21 C61 H61A 109.5 . . ?
H61B C61 H61A 109.5 . . ?
N21 C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
N22 C12 C22 118.17(19) . . ?
N22 C12 S12 125.02(17) . . ?
C22 C12 S12 116.79(16) . . ?
O22 C22 N12 122.35(19) . . ?
O22 C22 C12 118.93(18) . . ?
N12 C22 C12 118.64(19) . . ?
N12 C32 C42 109.8(2) . . ?
N12 C32 H32A 109.7 . . ?
C42 C32 H32A 109.7 . . ?
N12 C32 H32B 109.7 . . ?
C42 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
N22 C42 C32 110.6(2) . . ?
N22 C42 H42B 109.5 . . ?
C32 C42 H42B 109.5 . . ?
N22 C42 H42A 109.5 . . ?
C32 C42 H42A 109.5 . . ?
H42B C42 H42A 108.1 . . ?
N12 C52 H52B 109.5 . . ?
N12 C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N12 C52 H52A 109.5 . . ?
H52B C52 H52A 109.5 . . ?
H52C C52 H52A 109.5 . . ?
N22 C62 H62A 109.5 . . ?
N22 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
N22 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62C C62 H62B 109.5 . . ?
C21 N11 C51 121.01(19) . . ?
C21 N11 C31 121.24(19) . . ?
C51 N11 C31 117.46(19) . . ?
C11 N21 C61 121.9(2) . . ?
C11 N21 C41 119.7(2) . . ?
C61 N21 C41 118.3(2) . . ?
C22 N12 C32 120.68(19) . . ?
C22 N12 C52 120.3(2) . . ?
C32 N12 C52 118.6(2) . . ?
C12 N22 C62 121.86(19) . . ?
C12 N22 C42 119.66(19) . . ?
C62 N22 C42 118.33(19) . . ?
F6 B F4 82.9(11) . . ?
F6 B F2 125.0(10) . . ?
F4 B F2 116.5(6) . . ?
F6 B F5 122.7(13) . . ?
F4 B F5 142.3(8) . . ?
F2 B F5 73.7(8) . . ?
F6 B F3 97.1(10) . . ?
F4 B F3 110.9(6) . . ?
F2 B F3 118.4(7) . . ?
F5 B F3 44.9(8) . . ?
F6 B F8 113.7(11) . . ?
F4 B F8 80.5(10) . . ?
F2 B F8 37.3(9) . . ?
F5 B F8 108.3(12) . . ?
F3 B F8 148.5(8) . . ?
F6 B F7 119.6(12) . . ?
F4 B F7 44.0(5) . . ?
F2 B F7 106.4(7) . . ?
F5 B F7 98.8(8) . . ?
F3 B F7 82.2(6) . . ?
F8 B F7 87.8(11) . . ?
F6 B F1 26.5(11) . . ?
F4 B F1 104.7(6) . . ?
F2 B F1 101.1(6) . . ?
F5 B F1 108.6(6) . . ?
F3 B F1 102.6(5) . . ?
F8 B F1 102.5(8) . . ?
F7 B F1 145.6(7) . . ?
C11 S11 Fe 99.42(8) . . ?
C12 S12 Fe 98.56(8) . . ?
O22 Fe O21 80.72(6) . . ?
O22 Fe Cl2 93.53(5) . . ?
O21 Fe Cl2 165.22(4) . . ?
O22 Fe Cl1 166.04(4) . . ?
O21 Fe Cl1 93.23(5) . . ?
Cl2 Fe Cl1 95.19(2) . . ?
O22 Fe S12 80.08(4) . . ?
O21 Fe S12 87.37(4) . . ?
Cl2 Fe S12 105.15(3) . . ?
Cl1 Fe S12 87.13(2) . . ?
O22 Fe S11 89.35(5) . . ?
O21 Fe S11 78.13(4) . . ?
Cl2 Fe S11 88.26(2) . . ?
Cl1 Fe S11 101.78(3) . . ?
S12 Fe S11 163.30(2) . . ?
C21 O21 Fe 123.18(13) . . ?
C22 O22 Fe 121.97(13) . . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.182
_refine_diff_density_rms         0.055
####################################################################### 
# 
# 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_fe106s1_compound-3
_database_code_depnum_ccdc_archive 'CCDC 1037917'
_audit_update_record             
;
2014-12-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H10 Fe N6 O S5 1-, C24 H20 P 1+'
_chemical_formula_sum            'C34 H30 Fe N6 O P S5'
_chemical_formula_weight         785.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc
_symmetry_space_group_name_Hall  'C -2yc'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   9.59(1)
_cell_length_b                   31.06(2)
_cell_length_c                   12.91(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.82(3)
_cell_angle_gamma                90.00
_cell_volume                     3810(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24
_cell_measurement_theta_min      6.23
_cell_measurement_theta_max      13.15

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1620
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
local program based on Walker & Stuart,
(a) Walker, N.; Stuart, D. Acta Crystallogr., Sect. A 1983, 39, 158;
(b) Ugozzoli, F. Comput. Chem. 1987, 11, 109
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Philips PW 1100 diffractometer'
_diffrn_measurement_method       Theta-2theta
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         1
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4292
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0795
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.01
_reflns_number_total             4292
_reflns_number_gt                2665
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'local program'
_computing_cell_refinement       'local program'
_computing_data_reduction        'local program'
_computing_structure_solution    Sir97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep3 for windows'
_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)+(0.0760P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_number_reflns         4292
_refine_ls_number_parameters     435
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1470
_refine_ls_wR_factor_gt          0.1305
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.006
_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
C11 C 0.4659(9) 0.2870(2) 0.3574(7) 0.052(2) Uani 1 1 d . . .
C12 C 0.0681(8) 0.2248(3) 0.4247(7) 0.051(2) Uani 1 1 d . . .
C13 C 0.0128(8) 0.3460(3) 0.5975(7) 0.060(2) Uani 1 1 d . . .
C14 C -0.0463(8) 0.3154(2) 0.1992(9) 0.055(2) Uani 1 1 d . . .
C15 C 0.1666(8) 0.4171(3) 0.3418(7) 0.0490(19) Uani 1 1 d . . .
C16 C 0.6068(7) 0.4351(2) 0.2545(5) 0.0375(16) Uani 1 1 d . . .
C17 C 0.3975(7) 0.4255(2) 0.0658(6) 0.0402(17) Uani 1 1 d . . .
C18 C 0.4727(7) 0.5110(2) 0.1498(6) 0.0388(17) Uani 1 1 d . . .
C19 C 0.6775(8) 0.4599(2) 0.0488(6) 0.0434(18) Uani 1 1 d . . .
C21 C 0.4658(8) 0.2973(2) 0.4712(6) 0.0424(17) Uani 1 1 d . . .
C26 C 0.7367(8) 0.4147(3) 0.2692(6) 0.051(2) Uani 1 1 d . . .
H26 H 0.7949 0.4144 0.2171 0.061 Uiso 1 1 calc R . .
C27 C 0.3353(9) 0.3943(2) 0.1212(6) 0.0481(19) Uani 1 1 d . . .
H27 H 0.3686 0.3889 0.1911 0.058 Uiso 1 1 calc R . .
C28 C 0.5573(9) 0.5394(2) 0.2139(7) 0.053(2) Uani 1 1 d . . .
H28 H 0.6443 0.5309 0.2485 0.063 Uiso 1 1 calc R . .
C29 C 0.7082(8) 0.4220(3) -0.0018(7) 0.053(2) Uani 1 1 d . . .
H29 H 0.6578 0.3970 0.0070 0.063 Uiso 1 1 calc R . .
C31 C 0.6887(12) 0.2614(4) 0.5037(13) 0.111(5) Uani 1 1 d . . .
H31A H 0.7748 0.2669 0.5505 0.134 Uiso 1 1 calc R . .
H31B H 0.6663 0.2311 0.5088 0.134 Uiso 1 1 calc R . .
C36 C 0.7761(10) 0.3949(3) 0.3646(7) 0.064(2) Uani 1 1 d . . .
H36 H 0.8630 0.3811 0.3764 0.077 Uiso 1 1 calc R . .
C37 C 0.2228(9) 0.3715(3) 0.0706(8) 0.061(2) Uani 1 1 d . . .
H37 H 0.1807 0.3503 0.1067 0.074 Uiso 1 1 calc R . .
C38 C 0.5067(13) 0.5818(3) 0.2245(8) 0.069(3) Uani 1 1 d . . .
H38 H 0.5636 0.6018 0.2635 0.083 Uiso 1 1 calc R . .
C39 C 0.8142(10) 0.4217(3) -0.0653(8) 0.076(3) Uani 1 1 d . . .
H39 H 0.8334 0.3969 -0.1014 0.091 Uiso 1 1 calc R . .
C41 C 0.7115(12) 0.2709(5) 0.3982(15) 0.127(6) Uani 1 1 d . . .
H41A H 0.7698 0.2485 0.3741 0.152 Uiso 1 1 calc R . .
H41B H 0.7624 0.2979 0.3978 0.152 Uiso 1 1 calc R . .
C46 C 0.6916(10) 0.3946(3) 0.4428(7) 0.061(2) Uani 1 1 d . . .
H46 H 0.7216 0.3809 0.5060 0.073 Uiso 1 1 calc R . .
C47 C 0.1712(8) 0.3795(3) -0.0340(8) 0.060(2) Uani 1 1 d . . .
H47 H 0.0932 0.3647 -0.0666 0.072 Uiso 1 1 calc R . .
C48 C 0.3766(11) 0.5937(3) 0.1788(8) 0.067(3) Uani 1 1 d . . .
H48 H 0.3440 0.6214 0.1888 0.080 Uiso 1 1 calc R . .
C49 C 0.8921(10) 0.4597(4) -0.0740(9) 0.080(3) Uani 1 1 d . . .
H49 H 0.9650 0.4601 -0.1147 0.096 Uiso 1 1 calc R . .
C51 C 0.5767(14) 0.2947(4) 0.6517(8) 0.101(4) Uani 1 1 d . . .
H51A H 0.4826 0.3000 0.6659 0.152 Uiso 1 1 calc R . .
H51B H 0.6348 0.3191 0.6728 0.152 Uiso 1 1 calc R . .
H51C H 0.6137 0.2697 0.6899 0.152 Uiso 1 1 calc R . .
C56 C 0.5635(9) 0.4147(3) 0.4271(6) 0.051(2) Uani 1 1 d . . .
H56 H 0.5058 0.4142 0.4794 0.062 Uiso 1 1 calc R . .
C57 C 0.2361(8) 0.4092(3) -0.0873(7) 0.054(2) Uani 1 1 d . . .
H57 H 0.2044 0.4139 -0.1577 0.065 Uiso 1 1 calc R . .
C58 C 0.2933(10) 0.5651(3) 0.1183(7) 0.058(2) Uani 1 1 d . . .
H58 H 0.2051 0.5738 0.0862 0.070 Uiso 1 1 calc R . .
C59 C 0.8609(10) 0.4950(3) -0.0237(10) 0.087(4) Uani 1 1 d . . .
H59 H 0.9143 0.5197 -0.0293 0.105 Uiso 1 1 calc R . .
C66 C 0.5195(8) 0.4355(2) 0.3340(6) 0.0460(18) Uani 1 1 d . . .
H66 H 0.4334 0.4497 0.3239 0.055 Uiso 1 1 calc R . .
C67 C 0.3494(8) 0.4328(3) -0.0383(6) 0.0491(19) Uani 1 1 d . . .
H67 H 0.3925 0.4534 -0.0755 0.059 Uiso 1 1 calc R . .
C68 C 0.3377(8) 0.5235(2) 0.1040(7) 0.052(2) Uani 1 1 d . . .
H68 H 0.2790 0.5041 0.0645 0.062 Uiso 1 1 calc R . .
C69 C 0.7526(9) 0.4966(3) 0.0364(8) 0.065(3) Uani 1 1 d . . .
H69 H 0.7309 0.5222 0.0679 0.078 Uiso 1 1 calc R . .
N11 N 0.5751(8) 0.2870(2) 0.5367(6) 0.0618(19) Uani 1 1 d . . .
N12 N 0.1256(8) 0.2571(2) 0.4303(6) 0.067(2) Uani 1 1 d . . .
N13 N 0.0629(8) 0.3362(2) 0.5260(6) 0.064(2) Uani 1 1 d . . .
N14 N 0.0114(8) 0.3189(2) 0.2807(6) 0.0564(19) Uani 1 1 d . . .
N15 N 0.1935(7) 0.3822(2) 0.3701(5) 0.0543(17) Uani 1 1 d . . .
N21 N 0.5818(10) 0.2742(2) 0.3257(7) 0.079(3) Uani 1 1 d . . .
O21 O 0.3593(5) 0.31563(16) 0.5057(5) 0.0586(17) Uani 1 1 d . . .
S11 S 0.3258(3) 0.29584(10) 0.2774(3) 0.0880(8) Uani 1 1 d . . .
S12 S -0.0164(3) 0.17970(7) 0.4166(3) 0.0817(8) Uani 1 1 d . . .
S13 S -0.0577(4) 0.35941(17) 0.6984(3) 0.1361(17) Uani 1 1 d . . .
S14 S -0.1280(3) 0.31171(10) 0.0795(2) 0.0897(9) Uani 1 1 d . . .
S15 S 0.1332(3) 0.46583(8) 0.3010(3) 0.0898(10) Uani 1 1 d . . .
Fe Fe 0.16429(9) 0.31997(3) 0.40296(8) 0.0409(3) Uani 1 1 d . . .
P P 0.53902(19) 0.45772(6) 0.13011(15) 0.0372(4) Uani 1 1 d . . .
C61 C 0.586(3) 0.2650(6) 0.2128(13) 0.197(10) Uani 1 1 d . . .
H61A H 0.5270 0.2853 0.1711 0.295 Uiso 1 1 calc R . .
H61B H 0.5517 0.2364 0.1969 0.295 Uiso 1 1 calc R . .
H61C H 0.6806 0.2675 0.1978 0.295 Uiso 1 1 calc R . .


_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
C11 N21 1.299(11) . ?
C11 C21 1.503(12) . ?
C11 S11 1.603(9) . ?
C12 N12 1.141(10) . ?
C12 S12 1.615(9) . ?
C13 N13 1.138(10) . ?
C13 S13 1.603(10) . ?
C14 N14 1.126(11) . ?
C14 S14 1.639(11) . ?
C15 N15 1.161(10) . ?
C15 S15 1.621(9) . ?
C16 C26 1.387(10) . ?
C16 C66 1.410(10) . ?
C16 P 1.793(7) . ?
C17 C67 1.380(11) . ?
C17 C27 1.387(10) . ?
C17 P 1.796(8) . ?
C18 C28 1.393(11) . ?
C18 C68 1.403(11) . ?
C18 P 1.803(7) . ?
C19 C69 1.369(11) . ?
C19 C29 1.399(11) . ?
C19 P 1.803(7) . ?
C21 N11 1.293(10) . ?
C21 O21 1.300(9) . ?
C26 C36 1.383(12) . ?
C26 H26 0.9300 . ?
C27 C37 1.379(12) . ?
C27 H27 0.9300 . ?
C28 C38 1.415(12) . ?
C28 H28 0.9300 . ?
C29 C39 1.391(11) . ?
C29 H29 0.9300 . ?
C31 C41 1.44(2) . ?
C31 N11 1.459(13) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C36 C46 1.378(12) . ?
C36 H36 0.9300 . ?
C37 C47 1.396(13) . ?
C37 H37 0.9300 . ?
C38 C48 1.357(14) . ?
C38 H38 0.9300 . ?
C39 C49 1.410(14) . ?
C39 H39 0.9300 . ?
C41 N21 1.454(17) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C46 C56 1.367(12) . ?
C46 H46 0.9300 . ?
C47 C57 1.351(12) . ?
C47 H47 0.9300 . ?
C48 C58 1.366(13) . ?
C48 H48 0.9300 . ?
C49 C59 1.329(15) . ?
C49 H49 0.9300 . ?
C51 N11 1.502(13) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C56 C66 1.380(11) . ?
C56 H56 0.9300 . ?
C57 C67 1.389(12) . ?
C57 H57 0.9300 . ?
C58 C68 1.380(10) . ?
C58 H58 0.9300 . ?
C59 C69 1.379(12) . ?
C59 H59 0.9300 . ?
C66 H66 0.9300 . ?
C67 H67 0.9300 . ?
C68 H68 0.9300 . ?
C69 H69 0.9300 . ?
N12 Fe 2.028(7) . ?
N13 Fe 2.035(8) . ?
N14 Fe 2.003(8) . ?
N15 Fe 2.007(7) . ?
N21 C61 1.490(17) . ?
O21 Fe 2.145(6) . ?
S11 Fe 2.504(4) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 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
N21 C11 C21 119.2(8) . . ?
N21 C11 S11 121.8(8) . . ?
C21 C11 S11 118.8(6) . . ?
N12 C12 S12 178.8(7) . . ?
N13 C13 S13 179.5(10) . . ?
N14 C14 S14 178.3(9) . . ?
N15 C15 S15 178.4(7) . . ?
C26 C16 C66 121.1(7) . . ?
C26 C16 P 120.7(5) . . ?
C66 C16 P 118.0(5) . . ?
C67 C17 C27 120.5(7) . . ?
C67 C17 P 119.3(6) . . ?
C27 C17 P 120.1(6) . . ?
C28 C18 C68 120.3(7) . . ?
C28 C18 P 118.5(5) . . ?
C68 C18 P 121.2(6) . . ?
C69 C19 C29 120.0(7) . . ?
C69 C19 P 122.7(6) . . ?
C29 C19 P 117.3(6) . . ?
N11 C21 O21 119.2(8) . . ?
N11 C21 C11 118.6(7) . . ?
O21 C21 C11 122.2(7) . . ?
C36 C26 C16 117.1(7) . . ?
C36 C26 H26 121.4 . . ?
C16 C26 H26 121.4 . . ?
C37 C27 C17 118.6(8) . . ?
C37 C27 H27 120.7 . . ?
C17 C27 H27 120.7 . . ?
C18 C28 C38 117.8(8) . . ?
C18 C28 H28 121.1 . . ?
C38 C28 H28 121.1 . . ?
C39 C29 C19 119.9(8) . . ?
C39 C29 H29 120.1 . . ?
C19 C29 H29 120.1 . . ?
C41 C31 N11 112.3(11) . . ?
C41 C31 H31A 109.1 . . ?
N11 C31 H31A 109.1 . . ?
C41 C31 H31B 109.1 . . ?
N11 C31 H31B 109.1 . . ?
H31A C31 H31B 107.9 . . ?
C46 C36 C26 122.6(8) . . ?
C46 C36 H36 118.7 . . ?
C26 C36 H36 118.7 . . ?
C27 C37 C47 121.2(8) . . ?
C27 C37 H37 119.4 . . ?
C47 C37 H37 119.4 . . ?
C48 C38 C28 121.3(9) . . ?
C48 C38 H38 119.4 . . ?
C28 C38 H38 119.4 . . ?
C29 C39 C49 118.6(9) . . ?
C29 C39 H39 120.7 . . ?
C49 C39 H39 120.7 . . ?
C31 C41 N21 113.4(9) . . ?
C31 C41 H41A 108.9 . . ?
N21 C41 H41A 108.9 . . ?
C31 C41 H41B 108.9 . . ?
N21 C41 H41B 108.9 . . ?
H41A C41 H41B 107.7 . . ?
C56 C46 C36 119.6(8) . . ?
C56 C46 H46 120.2 . . ?
C36 C46 H46 120.2 . . ?
C57 C47 C37 119.2(8) . . ?
C57 C47 H47 120.4 . . ?
C37 C47 H47 120.4 . . ?
C38 C48 C58 120.2(8) . . ?
C38 C48 H48 119.9 . . ?
C58 C48 H48 119.9 . . ?
C59 C49 C39 119.7(8) . . ?
C59 C49 H49 120.1 . . ?
C39 C49 H49 120.1 . . ?
N11 C51 H51A 109.5 . . ?
N11 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N11 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C46 C56 C66 120.3(8) . . ?
C46 C56 H56 119.8 . . ?
C66 C56 H56 119.8 . . ?
C47 C57 C67 120.9(8) . . ?
C47 C57 H57 119.5 . . ?
C67 C57 H57 119.5 . . ?
C48 C58 C68 121.2(8) . . ?
C48 C58 H58 119.4 . . ?
C68 C58 H58 119.4 . . ?
C49 C59 C69 122.8(9) . . ?
C49 C59 H59 118.6 . . ?
C69 C59 H59 118.6 . . ?
C56 C66 C16 119.2(7) . . ?
C56 C66 H66 120.4 . . ?
C16 C66 H66 120.4 . . ?
C17 C67 C57 119.6(7) . . ?
C17 C67 H67 120.2 . . ?
C57 C67 H67 120.2 . . ?
C58 C68 C18 119.2(8) . . ?
C58 C68 H68 120.4 . . ?
C18 C68 H68 120.4 . . ?
C19 C69 C59 118.9(8) . . ?
C19 C69 H69 120.5 . . ?
C59 C69 H69 120.5 . . ?
C21 N11 C31 121.0(9) . . ?
C21 N11 C51 120.4(8) . . ?
C31 N11 C51 117.8(10) . . ?
C12 N12 Fe 158.9(7) . . ?
C13 N13 Fe 176.4(8) . . ?
C14 N14 Fe 162.3(7) . . ?
C15 N15 Fe 159.1(7) . . ?
C11 N21 C41 120.8(10) . . ?
C11 N21 C61 120.2(14) . . ?
C41 N21 C61 118.9(13) . . ?
C21 O21 Fe 118.4(5) . . ?
C11 S11 Fe 99.9(4) . . ?
N14 Fe N15 87.6(3) . . ?
N14 Fe N12 89.4(3) . . ?
N15 Fe N12 176.9(3) . . ?
N14 Fe N13 104.1(3) . . ?
N15 Fe N13 91.2(3) . . ?
N12 Fe N13 89.1(3) . . ?
N14 Fe O21 165.8(3) . . ?
N15 Fe O21 93.2(2) . . ?
N12 Fe O21 89.8(3) . . ?
N13 Fe O21 90.1(3) . . ?
N14 Fe S11 86.3(3) . . ?
N15 Fe S11 92.0(2) . . ?
N12 Fe S11 88.2(2) . . ?
N13 Fe S11 169.3(2) . . ?
O21 Fe S11 79.5(2) . . ?
C16 P C17 110.7(3) . . ?
C16 P C19 109.3(3) . . ?
C17 P C19 108.8(4) . . ?
C16 P C18 109.0(3) . . ?
C17 P C18 108.5(3) . . ?
C19 P C18 110.5(3) . . ?
N21 C61 H61A 109.5 . . ?
N21 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N21 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.01
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_feesai6
_database_code_depnum_ccdc_archive 'CCDC 1037918'
_audit_update_record             
;
2014-12-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H30 Fe N6 S6 3+, 5.4(I3 1-), 0.2(I 1-)'
_chemical_formula_sum            'C18 H30 Fe I5.60 N6 S6'
_chemical_formula_weight         1289.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1
_symmetry_space_group_name_Hall  -P1

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

_cell_length_a                   8.487(4)
_cell_length_b                   13.970(6)
_cell_length_c                   16.988(9)
_cell_angle_alpha                73.850(10)
_cell_angle_beta                 77.69(2)
_cell_angle_gamma                76.69(2)
_cell_volume                     1858.6(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    24
_cell_measurement_theta_min      7.06
_cell_measurement_theta_max      11.44

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1198
_exptl_absorpt_coefficient_mu    5.414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.457
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        'crystal decomposition'
_diffrn_reflns_number            5289
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.1138
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         24.04
_reflns_number_total             4449
_reflns_number_gt                1840
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for windows'
_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.
 Part of the I3- molecules were found disordered together with an isolated
 I- anion.
 The I- anion was refined with a site occupancy factor of 0.2, whereas the
 I3- fragment was additionally disordered in two position in a channel-like
 cavity and they were refined with site occupancy factors of 0.6 and 0.2,
 respectively.
;

_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)+(0.0750P)²+0.0000P] 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         4449
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.0796
_refine_ls_wR_factor_ref         0.2016
_refine_ls_wR_factor_gt          0.1780
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.543(3) 0.4797(12) 0.2601(10) 0.073(6) Uani 1 1 d . . .
C12 C 0.731(2) 0.0590(10) 0.4546(9) 0.056(5) Uani 1 1 d . . .
C13 C 1.023(3) 0.2186(13) 0.1590(10) 0.069(6) Uani 1 1 d . . .
C21 C 0.403(3) 0.4215(12) 0.3025(10) 0.067(5) Uani 1 1 d . . .
C22 C 0.757(2) 0.1401(11) 0.4898(11) 0.064(5) Uani 1 1 d . . .
C23 C 0.884(2) 0.2140(12) 0.1250(12) 0.058(5) Uani 1 1 d . . .
C31 C 0.224(3) 0.5833(13) 0.3020(17) 0.117(8) Uani 1 1 d . . .
H31A H 0.2435 0.6015 0.3497 0.140 Uiso 1 1 calc R . .
H31B H 0.1100 0.6103 0.2956 0.140 Uiso 1 1 calc R . .
C32 C 0.771(2) -0.0554(13) 0.5866(11) 0.081(6) Uani 1 1 d . . .
H32A H 0.8878 -0.0808 0.5844 0.098 Uiso 1 1 calc R . .
H32B H 0.7147 -0.1095 0.6208 0.098 Uiso 1 1 calc R . .
C33 C 1.076(3) 0.1783(19) 0.0020(12) 0.119(8) Uani 1 1 d . . .
H33A H 1.1129 0.1054 0.0151 0.143 Uiso 1 1 calc R . .
H33B H 1.0735 0.2010 -0.0573 0.143 Uiso 1 1 calc R . .
C41 C 0.329(3) 0.6291(14) 0.2280(15) 0.113(8) Uani 1 1 d . . .
H41A H 0.2927 0.6248 0.1789 0.135 Uiso 1 1 calc R . .
H41B H 0.3208 0.7002 0.2258 0.135 Uiso 1 1 calc R . .
C42 C 0.729(3) 0.0257(16) 0.6255(12) 0.120(8) Uani 1 1 d . . .
H42A H 0.7897 0.0096 0.6711 0.144 Uiso 1 1 calc R . .
H42B H 0.6129 0.0332 0.6486 0.144 Uiso 1 1 calc R . .
C51 C 0.627(2) 0.6371(13) 0.1805(13) 0.113(8) Uani 1 1 d . . .
H51A H 0.5795 0.7071 0.1617 0.169 Uiso 1 1 calc R . .
H51B H 0.6811 0.6100 0.1336 0.169 Uiso 1 1 calc R . .
H51C H 0.7054 0.6314 0.2156 0.169 Uiso 1 1 calc R . .
C52 C 0.730(2) -0.1166(12) 0.4707(11) 0.093(6) Uani 1 1 d . . .
H52A H 0.7350 -0.1784 0.5133 0.140 Uiso 1 1 calc R . .
H52B H 0.8218 -0.1229 0.4272 0.140 Uiso 1 1 calc R . .
H52C H 0.6299 -0.1033 0.4485 0.140 Uiso 1 1 calc R . .
C53 C 1.312(3) 0.2166(14) 0.1417(12) 0.094(7) Uani 1 1 d . . .
H53A H 1.4040 0.2125 0.0980 0.142 Uiso 1 1 calc R . .
H53B H 1.3305 0.1604 0.1884 0.142 Uiso 1 1 calc R . .
H53C H 1.2982 0.2789 0.1580 0.142 Uiso 1 1 calc R . .
C61 C 0.115(3) 0.4224(18) 0.3586(14) 0.126(8) Uani 1 1 d . . .
H61A H 0.0168 0.4719 0.3641 0.188 Uiso 1 1 calc R . .
H61B H 0.1359 0.3828 0.4126 0.188 Uiso 1 1 calc R . .
H61C H 0.1024 0.3788 0.3265 0.188 Uiso 1 1 calc R . .
C62 C 0.775(3) 0.2069(16) 0.6047(11) 0.126(9) Uani 1 1 d . . .
H62A H 0.7768 0.1829 0.6633 0.190 Uiso 1 1 calc R . .
H62B H 0.6837 0.2611 0.5949 0.190 Uiso 1 1 calc R . .
H62C H 0.8753 0.2311 0.5778 0.190 Uiso 1 1 calc R . .
N11 N 0.496(2) 0.5795(10) 0.2280(9) 0.082(5) Uani 1 1 d . . .
N12 N 0.7340(17) -0.0326(10) 0.5059(8) 0.068(4) Uani 1 1 d . . .
N13 N 1.170(2) 0.2137(11) 0.1134(11) 0.075(5) Uani 1 1 d . . .
N21 N 0.252(2) 0.4735(10) 0.3170(9) 0.071(4) Uani 1 1 d . . .
N22 N 0.7607(17) 0.1216(9) 0.5702(9) 0.072(4) Uani 1 1 d . . .
N23 N 0.908(2) 0.2023(12) 0.0475(11) 0.078(5) Uani 1 1 d . . .
S11 S 0.7323(6) 0.4174(3) 0.2536(3) 0.0722(14) Uani 1 1 d . . .
S12 S 0.7039(6) 0.0877(3) 0.3560(3) 0.0681(14) Uani 1 1 d . . .
S13 S 0.9971(6) 0.2199(3) 0.2589(3) 0.0690(14) Uani 1 1 d . . .
S21 S 0.4486(6) 0.2956(3) 0.3314(3) 0.0729(15) Uani 1 1 d . . .
S22 S 0.7659(6) 0.2569(3) 0.4255(3) 0.0759(15) Uani 1 1 d . . .
S23 S 0.6957(6) 0.2350(3) 0.1777(3) 0.0685(14) Uani 1 1 d . . .
Fe Fe 0.7236(3) 0.25115(16) 0.30191(14) 0.0611(8) Uani 1 1 d . . .
I1 I 0.5000 0.5000 0.5000 0.1345(10) Uani 1 2 d S . .
I2 I 0.7059(3) 0.64998(15) 0.40399(13) 0.1689(9) Uani 1 1 d . . .
I3 I 0.8451(3) 0.48905(14) 0.91946(14) 0.1756(10) Uani 1 1 d . . .
I4 I 0.5000 0.5000 1.0000 0.1382(11) Uani 1 2 d S . .
I6A I 0.6830(18) 0.9252(6) 0.1860(5) 0.175(4) Uani 0.60 1 d P . 1
I5A I 1.0297(14) 0.9248(4) 0.1911(4) 0.192(4) Uani 0.60 1 d P . 1
I7A I 0.3874(14) 0.9348(5) 0.1355(5) 0.182(4) Uani 0.60 1 d P . 1
I5C I 0.857(3) 0.833(2) 0.2492(17) 0.348(16) Uani 0.20 1 d P A 2
I7B I 0.586(5) 0.9214(15) 0.1661(13) 0.21(2) Uani 0.20 1 d P . 3
I6B I 0.921(4) 0.9140(16) 0.1950(16) 0.238(16) Uani 0.20 1 d P . 3
I5B I 1.266(3) 0.9304(11) 0.1521(8) 0.139(11) Uani 0.20 1 d P . 3
C63 C 0.779(3) 0.1933(15) 0.0136(12) 0.102(7) Uani 1 1 d . . .
H63A H 0.8181 0.1842 -0.0417 0.154 Uiso 1 1 calc R . .
H63B H 0.6965 0.2536 0.0117 0.154 Uiso 1 1 calc R . .
H63C H 0.7321 0.1358 0.0472 0.154 Uiso 1 1 calc R . .
C43 C 1.193(3) 0.2269(18) 0.0231(13) 0.112(8) Uani 1 1 d . . .
H43A H 1.3046 0.1967 0.0036 0.134 Uiso 1 1 calc R . .
H43B H 1.1765 0.2986 -0.0040 0.134 Uiso 1 1 calc R . .


_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
C11 N11 1.346(19) . ?
C11 C21 1.53(2) . ?
C11 S11 1.64(2) . ?
C12 N12 1.331(17) . ?
C12 C22 1.50(2) . ?
C12 S12 1.665(16) . ?
C13 N13 1.32(2) . ?
C13 C23 1.44(2) . ?
C13 S13 1.669(18) . ?
C21 N21 1.328(18) . ?
C21 S21 1.665(16) . ?
C22 N22 1.323(18) . ?
C22 S22 1.700(14) . ?
C23 N23 1.34(2) . ?
C23 S23 1.663(18) . ?
C31 N21 1.45(2) . ?
C31 C41 1.46(2) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 N12 1.404(19) . ?
C32 C42 1.41(2) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C43 1.48(2) . ?
C33 N23 1.48(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C41 N11 1.43(2) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 N22 1.45(2) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C51 N11 1.48(2) . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 N12 1.467(19) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 N13 1.40(2) . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C61 N21 1.45(2) . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 N22 1.51(2) . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
N13 C43 1.47(2) . ?
N23 C63 1.388(19) . ?
S11 Fe 2.251(5) . ?
S12 Fe 2.243(4) . ?
S13 Fe 2.258(6) . ?
S21 Fe 2.256(6) . ?
S22 Fe 2.230(5) . ?
S23 Fe 2.250(5) . ?
I1 I2 2.945(2) 2_666 ?
I1 I2 2.945(2) . ?
I3 I4 2.946(3) . ?
I4 I3 2.946(3) 2_667 ?
I6A I7A 2.784(12) . ?
I6A I5A 2.961(13) . ?
I5A I7A 3.004(9) 1_655 ?
I7A I5A 3.004(10) 1_455 ?
I7B I5B 2.75(4) 1_455 ?
I7B I6B 2.97(4) . ?
I6B I5B 2.91(3) . ?
I5B I7B 2.75(4) 1_655 ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?

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
N11 C11 C21 115.6(17) . . ?
N11 C11 S11 125.4(16) . . ?
C21 C11 S11 119.0(12) . . ?
N12 C12 C22 116.1(14) . . ?
N12 C12 S12 124.9(12) . . ?
C22 C12 S12 119.0(10) . . ?
N13 C13 C23 120.1(17) . . ?
N13 C13 S13 120.9(17) . . ?
C23 C13 S13 118.8(15) . . ?
N21 C21 C11 118.7(15) . . ?
N21 C21 S21 123.0(15) . . ?
C11 C21 S21 118.3(14) . . ?
N22 C22 C12 119.7(12) . . ?
N22 C22 S22 121.9(13) . . ?
C12 C22 S22 118.2(12) . . ?
N23 C23 C13 118.8(16) . . ?
N23 C23 S23 120.8(14) . . ?
C13 C23 S23 120.1(15) . . ?
N21 C31 C41 112.2(17) . . ?
N21 C31 H31A 109.2 . . ?
C41 C31 H31A 109.2 . . ?
N21 C31 H31B 109.2 . . ?
C41 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
N12 C32 C42 115.6(15) . . ?
N12 C32 H32A 108.4 . . ?
C42 C32 H32A 108.4 . . ?
N12 C32 H32B 108.4 . . ?
C42 C32 H32B 108.4 . . ?
H32A C32 H32B 107.4 . . ?
C43 C33 N23 112(2) . . ?
C43 C33 H33A 109.2 . . ?
N23 C33 H33A 109.2 . . ?
C43 C33 H33B 109.2 . . ?
N23 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
N11 C41 C31 111.2(17) . . ?
N11 C41 H41A 109.4 . . ?
C31 C41 H41A 109.4 . . ?
N11 C41 H41B 109.4 . . ?
C31 C41 H41B 109.4 . . ?
H41A C41 H41B 108.0 . . ?
C32 C42 N22 113.6(17) . . ?
C32 C42 H42A 108.8 . . ?
N22 C42 H42A 108.8 . . ?
C32 C42 H42B 108.8 . . ?
N22 C42 H42B 108.8 . . ?
H42A C42 H42B 107.7 . . ?
N11 C51 H51A 109.5 . . ?
N11 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N11 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N12 C52 H52A 109.5 . . ?
N12 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N12 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N13 C53 H53A 109.5 . . ?
N13 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
N13 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N21 C61 H61A 109.5 . . ?
N21 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
N21 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N22 C62 H62A 109.5 . . ?
N22 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
N22 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C11 N11 C41 123.7(17) . . ?
C11 N11 C51 117.2(17) . . ?
C41 N11 C51 118.6(16) . . ?
C12 N12 C32 122.9(14) . . ?
C12 N12 C52 117.5(14) . . ?
C32 N12 C52 118.6(13) . . ?
C13 N13 C53 123.9(18) . . ?
C13 N13 C43 121.9(16) . . ?
C53 N13 C43 113.0(17) . . ?
C21 N21 C61 121.2(16) . . ?
C21 N21 C31 120.5(16) . . ?
C61 N21 C31 117.8(18) . . ?
C22 N22 C42 120.6(15) . . ?
C22 N22 C62 118.4(13) . . ?
C42 N22 C62 120.5(16) . . ?
C23 N23 C63 120.6(17) . . ?
C23 N23 C33 120.9(17) . . ?
C63 N23 C33 117.4(18) . . ?
C11 S11 Fe 107.6(6) . . ?
C12 S12 Fe 107.6(5) . . ?
C13 S13 Fe 106.4(8) . . ?
C21 S21 Fe 107.2(8) . . ?
C22 S22 Fe 107.2(7) . . ?
C23 S23 Fe 106.5(7) . . ?
S22 Fe S12 87.99(17) . . ?
S22 Fe S23 175.7(2) . . ?
S12 Fe S23 89.28(18) . . ?
S22 Fe S11 90.11(18) . . ?
S12 Fe S11 176.8(2) . . ?
S23 Fe S11 92.76(18) . . ?
S22 Fe S21 94.1(2) . . ?
S12 Fe S21 89.99(19) . . ?
S23 Fe S21 89.19(19) . . ?
S11 Fe S21 87.54(19) . . ?
S22 Fe S13 90.2(2) . . ?
S12 Fe S13 94.91(19) . . ?
S23 Fe S13 86.76(19) . . ?
S11 Fe S13 87.7(2) . . ?
S21 Fe S13 173.60(18) . . ?
I2 I1 I2 180.00(9) 2_666 . ?
I3 I4 I3 180.000(1) . 2_667 ?
I7A I6A I5A 164.5(5) . . ?
I6A I5A I7A 160.9(3) . 1_655 ?
I6A I7A I5A 145.5(4) . 1_455 ?
I5B I7B I6B 175.4(11) 1_455 . ?
I5B I6B I7B 157.2(11) . . ?
I7B I5B I6B 161.3(9) 1_655 . ?
N23 C63 H63A 109.5 . . ?
N23 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
N23 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N13 C43 C33 109.8(18) . . ?
N13 C43 H43A 109.7 . . ?
C33 C43 H43A 109.7 . . ?
N13 C43 H43B 109.7 . . ?
C33 C43 H43B 109.7 . . ?
H43A C43 H43B 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.758
_diffrn_reflns_theta_full        24.04
_diffrn_measured_fraction_theta_full 0.758
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.153
_chemical_properties_physical    'slow crystal decomposition'
####################################################################### 
# 
# 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_coesa614
_database_code_depnum_ccdc_archive 'CCDC 1037919'
_audit_update_record             
;
2014-12-05 deposited with the CCDC.
2015-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C18 H30 Co N6 S6 3+), 2I2, 3(I 1-), 3(I3 1-)'
_chemical_formula_sum            'C36 H60 Co2 I14 N12 S12'
_chemical_formula_weight         2940.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.543(1)
_cell_length_b                   42.417(3)
_cell_length_c                   14.520(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.476(1)
_cell_angle_gamma                90.00
_cell_volume                     8086(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31010
_cell_measurement_theta_min      0.96
_cell_measurement_theta_max      26.60

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5392
_exptl_absorpt_coefficient_mu    6.100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Breeze CCD'
_diffrn_measurement_method       'theta & omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            49411
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         0.96
_diffrn_reflns_theta_max         26.60
_reflns_number_total             8379
_reflns_number_gt                6090
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Sir2004
_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.
 The iodine atoms showed a severe disorder concerning the various forms in 
 which it is present in the structure. In particular, the I3- anions were 
 found disordered in various positions, which occupy a channel like cavity. 
   

;

_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)+(0.1161P)²+39.9432P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_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         8379
_refine_ls_number_parameters     453
_refine_ls_number_restraints     46
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1999
_refine_ls_wR_factor_gt          0.1780
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.07162(3) -0.2500 0.0330(3) Uani 1 2 d S . .
Co2 Co 0.0000 -0.16318(3) -0.2500 0.0379(3) Uani 1 2 d S . .
S21 S 0.16179(13) 0.06908(4) -0.13289(13) 0.0420(4) Uani 1 1 d . . .
S11 S 0.03458(13) 0.03625(4) -0.34391(14) 0.0447(4) Uani 1 1 d . A .
S12 S -0.03066(15) 0.10921(4) -0.15854(14) 0.0445(4) Uani 1 1 d . . .
S13 S 0.06019(15) -0.12779(4) -0.32501(14) 0.0449(4) Uani 1 1 d . . .
S14 S 0.05594(17) -0.20053(5) -0.32156(16) 0.0533(5) Uani 1 1 d . . .
S23 S 0.14812(15) -0.16175(5) -0.11116(14) 0.0493(4) Uani 1 1 d . . .
N23 N 0.2524(5) -0.12001(17) -0.2880(5) 0.0559(16) Uani 1 1 d . . .
N11 N 0.3170(5) 0.03641(18) -0.1313(5) 0.0584(17) Uani 1 1 d D . .
C11 C 0.1600(5) 0.02847(16) -0.2809(5) 0.0409(15) Uani 1 1 d . . .
C23 C 0.2277(6) -0.14247(17) -0.1497(6) 0.0468(16) Uani 1 1 d . . .
C12 C -0.0189(6) 0.14359(17) -0.2084(5) 0.0463(16) Uani 1 1 d . . .
C13 C 0.1861(6) -0.13004(15) -0.2555(5) 0.0418(15) Uani 1 1 d . . .
C21 C 0.2195(5) 0.04360(16) -0.1801(5) 0.0391(14) Uani 1 1 d . A .
N12 N -0.0407(7) 0.17025(18) -0.1796(6) 0.070(2) Uani 1 1 d . . .
N21 N 0.2036(5) 0.00824(18) -0.3173(5) 0.0604(18) Uani 1 1 d D A .
N13 N 0.3219(6) -0.13759(19) -0.0873(5) 0.0633(18) Uani 1 1 d . . .
C61 C 0.1452(9) -0.0087(3) -0.4125(7) 0.080(3) Uani 1 1 d . . .
H61A H 0.0906 -0.0200 -0.4071 0.120 Uiso 1 1 calc R A .
H61B H 0.1890 -0.0233 -0.4251 0.120 Uiso 1 1 calc R . .
H61C H 0.1178 0.0061 -0.4678 0.120 Uiso 1 1 calc R . .
C14 C 0.0316(6) -0.23527(18) -0.2791(6) 0.0533(19) Uani 1 1 d . . .
C43 C 0.3602(7) -0.1282(3) -0.2312(8) 0.075(3) Uani 1 1 d . . .
H43A H 0.4009 -0.1160 -0.2567 0.090 Uiso 1 1 calc R . .
H43B H 0.3703 -0.1504 -0.2399 0.090 Uiso 1 1 calc R . .
C33 C 0.3924(8) -0.1210(3) -0.1209(8) 0.080(3) Uani 1 1 d . . .
H33A H 0.4617 -0.1282 -0.0810 0.096 Uiso 1 1 calc R . .
H33B H 0.3899 -0.0985 -0.1111 0.096 Uiso 1 1 calc R . .
C31 C 0.372(2) 0.0116(9) -0.159(2) 0.085(17) Uani 0.40(5) 1 d PD A 1
H31A H 0.4438 0.0165 -0.1343 0.102 Uiso 0.40(5) 1 calc PR A 1
H31B H 0.3643 -0.0089 -0.1333 0.102 Uiso 0.40(5) 1 calc PR A 1
C41 C 0.324(4) 0.0129(17) -0.260(4) 0.103(17) Uani 0.40(5) 1 d P A 1
H41A H 0.3548 -0.0029 -0.2859 0.124 Uiso 0.40(5) 1 calc PR A 1
H41B H 0.3395 0.0332 -0.2800 0.124 Uiso 0.40(5) 1 calc PR A 1
C41A C 0.3050(10) -0.0047(5) -0.2561(15) 0.053(6) Uani 0.60(5) 1 d PD A 2
H41C H 0.3352 -0.0121 -0.3001 0.064 Uiso 0.60(5) 1 calc PR A 2
H41D H 0.3005 -0.0224 -0.2158 0.064 Uiso 0.60(5) 1 calc PR A 2
C31A C 0.3693(14) 0.0212(6) -0.187(2) 0.066(8) Uani 0.60(5) 1 d PD A 2
H31C H 0.4336 0.0124 -0.1388 0.079 Uiso 0.60(5) 1 calc PR A 2
H31D H 0.3838 0.0369 -0.2278 0.079 Uiso 0.60(5) 1 calc PR A 2
N14 N 0.0669(7) -0.26209(16) -0.2941(6) 0.071(2) Uani 1 1 d . . .
C32 C -0.0839(10) 0.1717(3) -0.1045(9) 0.087(3) Uani 1 1 d . . .
H32A H -0.1520 0.1634 -0.1345 0.131 Uiso 1 1 calc R . .
H32B H -0.0852 0.1932 -0.0845 0.131 Uiso 1 1 calc R . .
H32C H -0.0426 0.1594 -0.0457 0.131 Uiso 1 1 calc R . .
C51 C 0.3789(7) 0.0492(3) -0.0292(7) 0.077(3) Uani 1 1 d . A .
H51A H 0.3573 0.0703 -0.0250 0.115 Uiso 1 1 calc R . .
H51B H 0.4493 0.0493 -0.0167 0.115 Uiso 1 1 calc R . .
H51C H 0.3705 0.0363 0.0210 0.115 Uiso 1 1 calc R . .
C63 C 0.2167(9) -0.1050(3) -0.3912(8) 0.080(3) Uani 1 1 d . . .
H63A H 0.1591 -0.1163 -0.4395 0.120 Uiso 1 1 calc R . .
H63B H 0.2707 -0.1054 -0.4124 0.120 Uiso 1 1 calc R . .
H63C H 0.1975 -0.0835 -0.3876 0.120 Uiso 1 1 calc R . .
C53 C 0.3605(9) -0.1455(3) 0.0205(7) 0.095(4) Uani 1 1 d . . .
H53A H 0.3049 -0.1462 0.0395 0.143 Uiso 1 1 calc R . .
H53B H 0.4085 -0.1297 0.0605 0.143 Uiso 1 1 calc R . .
H53C H 0.3935 -0.1657 0.0327 0.143 Uiso 1 1 calc R . .
C34 C 0.1355(11) -0.2630(3) -0.3449(11) 0.106(4) Uani 1 1 d . . .
H34A H 0.1215 -0.2453 -0.3902 0.159 Uiso 1 1 calc R . .
H34B H 0.1246 -0.2822 -0.3832 0.159 Uiso 1 1 calc R . .
H34C H 0.2049 -0.2621 -0.2945 0.159 Uiso 1 1 calc R . .
C24 C 0.0511(10) -0.2907(2) -0.2511(9) 0.096(4) Uani 1 1 d . . .
H24A H 0.1041 -0.2931 -0.1823 0.115 Uiso 1 1 calc R . .
H24B H 0.0554 -0.3084 -0.2912 0.115 Uiso 1 1 calc R . .
C22 C -0.0388(13) 0.2002(2) -0.2315(10) 0.102(4) Uani 1 1 d . . .
H22A H -0.1048 0.2035 -0.2885 0.122 Uiso 1 1 calc R . .
H22B H -0.0265 0.2176 -0.1842 0.122 Uiso 1 1 calc R . .
I1 I 0.2165(3) 0.18966(8) 0.0293(2) 0.1059(10) Uani 0.551(8) 1 d P B 3
I2 I 0.2916(2) 0.15266(6) -0.09506(18) 0.0661(6) Uani 0.551(8) 1 d P B 3
I3 I 0.3640(2) 0.11772(6) -0.22375(18) 0.0739(7) Uani 0.551(8) 1 d P B 3
I1A I 0.2510(10) 0.19507(18) 0.0357(7) 0.267(5) Uani 0.449(8) 1 d PD B 4
I2A I 0.3142(5) 0.14926(14) -0.1038(5) 0.167(3) Uani 0.449(8) 1 d PD B 4
I3A I 0.3427(4) 0.1084(2) -0.2536(7) 0.177(3) Uani 0.449(8) 1 d PD B 4
I5 I 0.3321(5) 0.04595(16) 0.5113(6) 0.1102(16) Uani 0.57(3) 1 d P C 5
I5B I 0.3367(8) 0.0489(4) 0.5395(16) 0.140(3) Uani 0.43(3) 1 d P C 6
I8 I 0.6023(7) 0.2230(2) 0.0929(12) 0.099(2) Uani 0.25 1 d PU D 7
I9 I 0.7500 0.2500 0.0000 0.0836(6) Uiso 0.50 2 d SPU E 8
I8A I 0.6292(15) 0.2276(4) 0.1249(14) 0.108(10) Uani 0.13 1 d PU F 9
I9A I 0.6848(6) 0.24129(15) 0.0487(6) 0.0555(14) Uiso 0.10 1 d PU . 10
I8B I 0.6407(8) 0.2310(3) 0.0752(7) 0.087(2) Uani 0.25 1 d PU G 11
I8C I 0.5000 0.2128(2) 0.2500 0.38(2) Uani 0.25 2 d SPU H 12
I8D I 0.434(2) 0.2084(2) 0.1777(18) 0.251(11) Uani 0.13 1 d PU . 13
I9B I 0.7825(3) 0.25343(7) -0.0238(2) 0.0343(6) Uiso 0.15 1 d PU . 14
I8E I 0.5779(17) 0.2170(2) 0.1545(16) 0.190(10) Uani 0.13 1 d PU I 15
I4 I 0.5000 0.05635(2) 0.2500 0.0613(2) Uani 1 2 d S . .
I6 I 0.09942(6) 0.048280(15) 0.33073(6) 0.0763(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
Co1 S11 2.2255(19) . ?
Co1 S11 2.2255(19) 2_554 ?
Co1 S21 2.2355(17) 2_554 ?
Co1 S21 2.2355(17) . ?
Co1 S12 2.2390(19) 2_554 ?
Co1 S12 2.2390(19) . ?
Co2 S23 2.230(2) 2_554 ?
Co2 S23 2.2298(19) . ?
Co2 S14 2.231(2) . ?
Co2 S14 2.231(2) 2_554 ?
Co2 S13 2.2420(19) . ?
Co2 S13 2.2420(19) 2_554 ?
S21 C21 1.683(7) . ?
S11 C11 1.684(7) . ?
S12 C12 1.670(7) . ?
S13 C13 1.671(8) . ?
S14 C14 1.692(8) . ?
S23 C23 1.696(8) . ?
N23 C13 1.314(9) . ?
N23 C43 1.465(12) . ?
N23 C63 1.500(11) . ?
N11 C21 1.321(9) . ?
N11 C51 1.468(11) . ?
N11 C31 1.478(19) . ?
N11 C31A 1.478(15) . ?
C11 N21 1.307(9) . ?
C11 C21 1.488(9) . ?
C23 N13 1.294(10) . ?
C23 C13 1.485(10) . ?
C12 N12 1.292(10) . ?
C12 C12 1.526(14) 2_554 ?
N12 C32 1.475(12) . ?
N12 C22 1.485(12) . ?
N21 C61 1.461(11) . ?
N21 C41A 1.462(12) . ?
N21 C41 1.60(6) . ?
N13 C53 1.456(12) . ?
N13 C33 1.488(12) . ?
C14 N14 1.304(10) . ?
C14 C14 1.494(18) 2_554 ?
C43 C33 1.494(15) . ?
C31 C41 1.32(5) . ?
C41A C31A 1.509(18) . ?
N14 C24 1.427(14) . ?
N14 C34 1.474(16) . ?
C24 C24 1.50(3) 2_554 ?
C22 C22 1.44(3) 2_554 ?
I1 I2 2.934(4) . ?
I2 I3 2.914(3) . ?
I2A I3A 2.947(10) . ?
I9A I9A 2.91(2) 7_655 ?
I8D I8D 2.16(6) 2_655 ?
I9B I9B 1.419(8) 7_655 ?
I6 I6 2.8331(15) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S11 Co1 S11 95.23(11) . 2_554 ?
S11 Co1 S21 86.71(7) . 2_554 ?
S11 Co1 S21 89.55(7) 2_554 2_554 ?
S11 Co1 S21 89.55(7) . . ?
S11 Co1 S21 86.71(7) 2_554 . ?
S21 Co1 S21 174.46(11) 2_554 . ?
S11 Co1 S12 87.79(7) . 2_554 ?
S11 Co1 S12 176.87(8) 2_554 2_554 ?
S21 Co1 S12 89.79(7) 2_554 2_554 ?
S21 Co1 S12 94.16(7) . 2_554 ?
S11 Co1 S12 176.87(8) . . ?
S11 Co1 S12 87.79(7) 2_554 . ?
S21 Co1 S12 94.16(7) 2_554 . ?
S21 Co1 S12 89.79(7) . . ?
S12 Co1 S12 89.21(10) 2_554 . ?
S23 Co2 S23 176.88(12) 2_554 . ?
S23 Co2 S14 90.13(8) 2_554 . ?
S23 Co2 S14 92.09(8) . . ?
S23 Co2 S14 92.09(8) 2_554 2_554 ?
S23 Co2 S14 90.13(8) . 2_554 ?
S14 Co2 S14 89.53(12) . 2_554 ?
S23 Co2 S13 88.27(7) 2_554 . ?
S23 Co2 S13 89.65(7) . . ?
S14 Co2 S13 87.27(7) . . ?
S14 Co2 S13 176.78(8) 2_554 . ?
S23 Co2 S13 89.65(7) 2_554 2_554 ?
S23 Co2 S13 88.27(7) . 2_554 ?
S14 Co2 S13 176.78(9) . 2_554 ?
S14 Co2 S13 87.27(7) 2_554 2_554 ?
S13 Co2 S13 95.93(11) . 2_554 ?
C21 S21 Co1 105.5(2) . . ?
C11 S11 Co1 106.0(2) . . ?
C12 S12 Co1 106.3(2) . . ?
C13 S13 Co2 102.9(2) . . ?
C14 S14 Co2 105.9(3) . . ?
C23 S23 Co2 104.2(3) . . ?
C13 N23 C43 119.6(7) . . ?
C13 N23 C63 120.3(7) . . ?
C43 N23 C63 119.3(7) . . ?
C21 N11 C51 120.4(7) . . ?
C21 N11 C31 126.9(11) . . ?
C51 N11 C31 111.7(11) . . ?
C21 N11 C31A 119.6(11) . . ?
C51 N11 C31A 118.7(10) . . ?
C31 N11 C31A 22(2) . . ?
N21 C11 C21 120.2(6) . . ?
N21 C11 S11 120.6(5) . . ?
C21 C11 S11 119.1(5) . . ?
N13 C23 C13 120.3(7) . . ?
N13 C23 S23 120.9(6) . . ?
C13 C23 S23 118.7(6) . . ?
N12 C12 C12 118.6(5) . 2_554 ?
N12 C12 S12 122.5(6) . . ?
C12 C12 S12 118.8(3) 2_554 . ?
N23 C13 C23 116.9(7) . . ?
N23 C13 S13 123.2(6) . . ?
C23 C13 S13 119.9(5) . . ?
N11 C21 C11 117.6(6) . . ?
N11 C21 S21 122.6(5) . . ?
C11 C21 S21 119.8(5) . . ?
C12 N12 C32 121.2(8) . . ?
C12 N12 C22 121.6(8) . . ?
C32 N12 C22 116.6(8) . . ?
C11 N21 C61 121.3(7) . . ?
C11 N21 C41A 122.6(8) . . ?
C61 N21 C41A 114.5(8) . . ?
C11 N21 C41 109(2) . . ?
C61 N21 C41 128(2) . . ?
C41A N21 C41 30.1(17) . . ?
C23 N13 C53 121.2(8) . . ?
C23 N13 C33 121.2(7) . . ?
C53 N13 C33 117.4(8) . . ?
N14 C14 C14 118.5(6) . 2_554 ?
N14 C14 S14 122.7(7) . . ?
C14 C14 S14 118.8(3) 2_554 . ?
N23 C43 C33 108.8(8) . . ?
N13 C33 C43 108.3(7) . . ?
C41 C31 N11 100(3) . . ?
C31 C41 N21 121(4) . . ?
N21 C41A C31A 107.8(17) . . ?
N11 C31A C41A 111.3(14) . . ?
C14 N14 C24 121.3(10) . . ?
C14 N14 C34 120.4(9) . . ?
C24 N14 C34 117.9(9) . . ?
N14 C24 C24 110.9(8) . 2_554 ?
C22 C22 N12 112.2(9) 2_554 . ?
I3 I2 I1 177.99(14) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.60
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.662
_refine_diff_density_min         -2.266
_refine_diff_density_rms         0.173




