# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 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_as51o
_database_code_depnum_ccdc_archive 'CCDC 1041514'
_audit_update_record             
;
2014-12-30 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXTL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19.50 H18.50 As3 Cl6.50 S6'
_chemical_formula_weight         900.39

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'
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   20.703(4)
_cell_length_b                   9.885(2)
_cell_length_c                   14.702(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3008.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    1230
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      15.68

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1764
_exptl_absorpt_coefficient_mu    4.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5830
_exptl_absorpt_correction_T_max  0.8462
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28227
_diffrn_reflns_av_R_equivalents  0.1156
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2818
_reflns_number_gt                1744
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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. 

 In the crystal structure two solvent molecules, CHCl3 and C2Cl4 share 
 the same position and disordred over a mirror plane.  
 There solvent molecules were treated  by SQUEEZE 
 [Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.].  
 Corrections of the X-ray data by SQUEEZE is  306 electron; 
 the required values 276 electron for two CHCl3 and two C2Cl4 molecules
 in the full unit cell. 

;

_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)+(0.1156P)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         2818
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2100
_refine_ls_wR_factor_gt          0.1818
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
As1 As 0.36730(6) 0.2500 0.59620(8) 0.0525(4) Uani 1 2 d S . .
As2 As 0.21057(7) 0.2500 0.45298(9) 0.0755(6) Uani 1 2 d S . .
As3 As 0.37680(6) 0.2500 0.33136(8) 0.0577(5) Uani 1 2 d S . .
Cl1 Cl 0.47092(17) 0.2500 0.5557(3) 0.0787(12) Uani 1 2 d S . .
Cl2 Cl 0.18214(18) 0.2500 0.5999(2) 0.0741(11) Uani 1 2 d S . .
Cl3 Cl 0.3063(2) 0.2500 0.2169(3) 0.0844(13) Uani 1 2 d S . .
S1 S 0.36653(18) 0.0961(4) 0.70408(19) 0.1009(13) Uani 1 1 d . . .
S2 S 0.14438(15) 0.0949(6) 0.3962(2) 0.1278(19) Uani 1 1 d . . .
S3 S 0.44533(18) 0.0928(5) 0.2857(2) 0.1220(17) Uani 1 1 d . . .
C1 C 0.3456(6) -0.0593(9) 0.5464(7) 0.060(3) Uani 1 1 d . . .
C2 C 0.2776(6) -0.0567(10) 0.5353(8) 0.075(3) Uani 1 1 d . . .
H2A H 0.2506 -0.0531 0.5875 0.090 Uiso 1 1 calc R . .
C3 C 0.2506(6) -0.0594(10) 0.4519(9) 0.073(3) Uani 1 1 d . . .
C4 C 0.2884(6) -0.0581(10) 0.3765(9) 0.075(3) Uani 1 1 d . . .
H4A H 0.2690 -0.0547 0.3180 0.091 Uiso 1 1 calc R . .
C5 C 0.3535(6) -0.0615(9) 0.3841(7) 0.064(3) Uani 1 1 d . . .
C6 C 0.3823(6) -0.0580(9) 0.4707(7) 0.069(3) Uani 1 1 d . . .
H6A H 0.4280 -0.0548 0.4759 0.083 Uiso 1 1 calc R . .
C7 C 0.3755(6) -0.0573(14) 0.6432(7) 0.103(5) Uani 1 1 d . . .
H7A H 0.4222 -0.0775 0.6380 0.123 Uiso 1 1 calc R . .
H7B H 0.3555 -0.1308 0.6792 0.123 Uiso 1 1 calc R . .
C8 C 0.1762(7) -0.055(2) 0.4431(11) 0.164(9) Uani 1 1 d . . .
H8A H 0.1572 -0.0680 0.5043 0.197 Uiso 1 1 calc R . .
H8B H 0.1622 -0.1321 0.4049 0.197 Uiso 1 1 calc R . .
C9 C 0.3950(7) -0.0569(17) 0.3012(9) 0.120(6) Uani 1 1 d . . .
H9A H 0.3666 -0.0656 0.2474 0.144 Uiso 1 1 calc R . .
H9B H 0.4237 -0.1371 0.3021 0.144 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
As1 S1 2.198(3) 7_565 ?
As1 S1 2.198(3) . ?
As1 Cl1 2.226(4) . ?
As2 S2 2.219(4) 7_565 ?
As2 S2 2.219(4) . ?
As2 Cl2 2.239(4) . ?
As3 S3 2.208(3) . ?
As3 S3 2.209(3) 7_565 ?
As3 Cl3 2.227(4) . ?
S1 C7 1.770(14) . ?
S2 C8 1.76(2) . ?
S3 C9 1.824(17) . ?
C1 C6 1.347(14) . ?
C1 C2 1.419(15) . ?
C1 C7 1.552(14) . ?
C2 C3 1.347(14) . ?
C2 H2A 0.9500 . ?
C3 C4 1.357(15) . ?
C3 C8 1.546(19) . ?
C4 C5 1.353(15) . ?
C4 H4A 0.9500 . ?
C5 C6 1.406(13) . ?
C5 C9 1.491(16) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?

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
S1 As1 S1 87.6(2) 7_565 . ?
S1 As1 Cl1 101.54(14) 7_565 . ?
S1 As1 Cl1 101.54(14) . . ?
S2 As2 S2 87.4(3) 7_565 . ?
S2 As2 Cl2 101.58(12) 7_565 . ?
S2 As2 Cl2 101.59(12) . . ?
S3 As3 S3 89.4(3) . 7_565 ?
S3 As3 Cl3 101.04(14) . . ?
S3 As3 Cl3 101.04(14) 7_565 . ?
C7 S1 As1 103.1(4) . . ?
C8 S2 As2 101.7(4) . . ?
C9 S3 As3 99.6(4) . . ?
C6 C1 C2 117.7(10) . . ?
C6 C1 C7 122.2(11) . . ?
C2 C1 C7 120.1(11) . . ?
C3 C2 C1 121.1(11) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C2 C3 C4 120.2(12) . . ?
C2 C3 C8 119.3(13) . . ?
C4 C3 C8 120.4(12) . . ?
C5 C4 C3 120.5(12) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 119.7(11) . . ?
C4 C5 C9 120.4(11) . . ?
C6 C5 C9 119.7(12) . . ?
C1 C6 C5 120.6(11) . . ?
C1 C6 H6A 119.7 . . ?
C5 C6 H6A 119.7 . . ?
C1 C7 S1 115.7(8) . . ?
C1 C7 H7A 108.4 . . ?
S1 C7 H7A 108.4 . . ?
C1 C7 H7B 108.4 . . ?
S1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.4 . . ?
C3 C8 S2 115.4(10) . . ?
C3 C8 H8A 108.4 . . ?
S2 C8 H8A 108.4 . . ?
C3 C8 H8B 108.4 . . ?
S2 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C5 C9 S3 117.1(9) . . ?
C5 C9 H9A 108.0 . . ?
S3 C9 H9A 108.0 . . ?
C5 C9 H9B 108.0 . . ?
S3 C9 H9B 108.0 . . ?
H9A C9 H9B 107.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S1 As1 S1 C7 -174.1(4) 7_565 . . . ?
Cl1 As1 S1 C7 -72.8(5) . . . . ?
S2 As2 S2 C8 -171.8(6) 7_565 . . . ?
Cl2 As2 S2 C8 -70.5(6) . . . . ?
S3 As3 S3 C9 -172.4(5) 7_565 . . . ?
Cl3 As3 S3 C9 -71.2(5) . . . . ?
C6 C1 C2 C3 3.0(15) . . . . ?
C7 C1 C2 C3 -179.5(10) . . . . ?
C1 C2 C3 C4 -3.1(17) . . . . ?
C1 C2 C3 C8 -179.4(11) . . . . ?
C2 C3 C4 C5 3.6(17) . . . . ?
C8 C3 C4 C5 179.8(12) . . . . ?
C3 C4 C5 C6 -3.9(15) . . . . ?
C3 C4 C5 C9 -178.6(11) . . . . ?
C2 C1 C6 C5 -3.4(14) . . . . ?
C7 C1 C6 C5 179.3(9) . . . . ?
C4 C5 C6 C1 3.9(14) . . . . ?
C9 C5 C6 C1 178.6(10) . . . . ?
C6 C1 C7 S1 108.2(10) . . . . ?
C2 C1 C7 S1 -69.1(13) . . . . ?
As1 S1 C7 C1 -31.5(11) . . . . ?
C2 C3 C8 S2 111.2(12) . . . . ?
C4 C3 C8 S2 -65.0(16) . . . . ?
As2 S2 C8 C3 -36.2(13) . . . . ?
C4 C5 C9 S3 113.6(11) . . . . ?
C6 C5 C9 S3 -61.0(14) . . . . ?
As3 S3 C9 C5 -40.0(11) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.130
####################################################################### 
# 
# 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_as120
_database_code_depnum_ccdc_archive 'CCDC 1041515'
_audit_update_record             
;
2014-12-30 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXLTL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H24 Cl3 S6 Sb3'
_chemical_formula_weight         976.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   14.2066(8)
_cell_length_b                   14.2066(8)
_cell_length_c                   33.410(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5839.6(6)
_cell_formula_units_Z            6
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3186
_cell_measurement_theta_min      4.46
_cell_measurement_theta_max      65.57

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2808
_exptl_absorpt_coefficient_mu    21.393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0236
_exptl_absorpt_correction_T_max  0.6743
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6626
_diffrn_reflns_av_R_equivalents  0.1290
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         6.23
_diffrn_reflns_theta_max         65.82
_reflns_number_total             1134
_reflns_number_gt                928
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


_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. 

 In the crystal structure a solvent molecule C6H6 is 
 disordered over three positions and were treated 
 by SQUEEZE 
 [Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.].  
 Corrections of the X-ray data by SQUEEZE is  136 electron; 
 the required values 252 electron for six C6H6 molecules. 


;

_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)+(0.1006P)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         1134
_refine_ls_number_parameters     64
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1493
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Sb1 Sb 0.6964(14) 0.4988(8) 0.0855(6) 0.065(5) Uani 0.25 1 d P . .
Sb1A Sb 0.6398(8) 0.4721(6) 0.0864(4) 0.0324(11) Uani 0.25 1 d P . .
S1 S 0.66298(18) 0.60053(13) 0.03222(5) 0.0820(7) Uani 1 1 d . . .
Cl1 Cl 0.8928(2) 0.5837(3) 0.07958(17) 0.0655(11) Uani 0.50 1 d P . .
C1 C 0.7138(9) 0.5565(7) -0.0092(3) 0.094(3) Uani 1 1 d . . .
H1A H 0.6844 0.5687 -0.0343 0.113 Uiso 1 1 calc R . .
H1B H 0.7938 0.6038 -0.0101 0.113 Uiso 1 1 calc R . .
C2 C 0.6880(6) 0.4393(5) -0.00866(17) 0.0641(17) Uani 1 1 d . . .
C3 C 0.5826(6) 0.3530(6) -0.00879(18) 0.0656(17) Uani 1 1 d . . .
H3A H 0.5240 0.3673 -0.0090 0.079 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
Sb1 Sb1A 0.18(3) 18_654 ?
Sb1 Sb1A 0.698(7) . ?
Sb1 Sb1 0.75(3) 18_654 ?
Sb1 S1 2.368(14) 18_654 ?
Sb1 Cl1 2.431(17) . ?
Sb1 S1 2.483(16) . ?
Sb1 Cl1 2.806(17) 16_544 ?
Sb1A Sb1 0.18(3) 18_654 ?
Sb1A Sb1A 0.693(16) 18_654 ?
Sb1A S1 2.340(12) 18_654 ?
Sb1A Cl1 2.460(10) 18_654 ?
Sb1A S1 2.473(9) . ?
Sb1A Cl1 2.854(11) 2_655 ?
S1 C1 1.810(9) . ?
S1 Sb1A 2.340(12) 18_654 ?
S1 Sb1 2.368(14) 18_654 ?
Cl1 Cl1 0.648(5) 16_544 ?
Cl1 Sb1A 2.460(10) 18_654 ?
Cl1 Sb1 2.806(17) 16_544 ?
Cl1 Sb1A 2.854(11) 3_665 ?
C1 C2 1.515(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.354(10) 3_665 ?
C2 C3 1.382(10) . ?
C3 C2 1.354(10) 2_655 ?
C3 H3A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Sb1A Sb1 Sb1A 81(8) 18_654 . ?
Sb1A Sb1 Sb1 68(8) 18_654 18_654 ?
Sb1A Sb1 Sb1 14(2) . 18_654 ?
Sb1A Sb1 S1 124(5) 18_654 18_654 ?
Sb1A Sb1 S1 79.2(12) . 18_654 ?
Sb1 Sb1 S1 90(2) 18_654 18_654 ?
Sb1A Sb1 Cl1 97(8) 18_654 . ?
Sb1A Sb1 Cl1 176.6(14) . . ?
Sb1 Sb1 Cl1 164(3) 18_654 . ?
S1 Sb1 Cl1 104.2(6) 18_654 . ?
Sb1A Sb1 S1 36(4) 18_654 . ?
Sb1A Sb1 S1 81.1(10) . . ?
Sb1 Sb1 S1 73(2) 18_654 . ?
S1 Sb1 S1 89.5(3) 18_654 . ?
Cl1 Sb1 S1 99.1(6) . . ?
Sb1A Sb1 Cl1 104(8) 18_654 16_544 ?
Sb1A Sb1 Cl1 166.7(13) . 16_544 ?
Sb1 Sb1 Cl1 162.4(19) 18_654 16_544 ?
S1 Sb1 Cl1 107.3(6) 18_654 16_544 ?
Cl1 Sb1 Cl1 11.63(12) . 16_544 ?
S1 Sb1 Cl1 110.1(6) . 16_544 ?
Sb1 Sb1A Sb1A 84(8) 18_654 18_654 ?
Sb1 Sb1A Sb1 99(8) 18_654 . ?
Sb1A Sb1A Sb1 15(3) 18_654 . ?
Sb1 Sb1A S1 142(5) 18_654 18_654 ?
Sb1A Sb1A S1 92.9(17) 18_654 18_654 ?
Sb1 Sb1A S1 83.8(12) . 18_654 ?
Sb1 Sb1A Cl1 79(8) 18_654 18_654 ?
Sb1A Sb1A Cl1 163(2) 18_654 18_654 ?
Sb1 Sb1A Cl1 173.0(13) . 18_654 ?
S1 Sb1A Cl1 102.4(3) 18_654 18_654 ?
Sb1 Sb1A S1 53(5) 18_654 . ?
Sb1A Sb1A S1 70.9(15) 18_654 . ?
Sb1 Sb1A S1 82.7(10) . . ?
S1 Sb1A S1 90.4(2) 18_654 . ?
Cl1 Sb1A S1 100.3(4) 18_654 . ?
Sb1 Sb1A Cl1 73(8) 18_654 2_655 ?
Sb1A Sb1A Cl1 154(2) 18_654 2_655 ?
Sb1 Sb1A Cl1 161.9(12) . 2_655 ?
S1 Sb1A Cl1 113.0(3) 18_654 2_655 ?
Cl1 Sb1A Cl1 11.15(11) 18_654 2_655 ?
S1 Sb1A Cl1 102.9(4) . 2_655 ?
C1 S1 Sb1A 94.7(3) . 18_654 ?
C1 S1 Sb1 100.8(4) . 18_654 ?
Sb1A S1 Sb1 17.0(2) 18_654 18_654 ?
C1 S1 Sb1A 103.5(3) . . ?
Sb1A S1 Sb1A 16.2(4) 18_654 . ?
Sb1 S1 Sb1A 3.5(6) 18_654 . ?
C1 S1 Sb1 97.0(4) . . ?
Sb1A S1 Sb1 2.6(5) 18_654 . ?
Sb1 S1 Sb1 17.5(8) 18_654 . ?
Sb1A S1 Sb1 16.18(18) . . ?
Cl1 Cl1 Sb1 119.3(5) 16_544 . ?
Cl1 Cl1 Sb1A 121.6(4) 16_544 18_654 ?
Sb1 Cl1 Sb1A 4.2(7) . 18_654 ?
Cl1 Cl1 Sb1 49.1(4) 16_544 16_544 ?
Sb1 Cl1 Sb1 79.0(4) . 16_544 ?
Sb1A Cl1 Sb1 79.49(11) 18_654 16_544 ?
Cl1 Cl1 Sb1A 47.2(3) 16_544 3_665 ?
Sb1 Cl1 Sb1A 78.99(12) . 3_665 ?
Sb1A Cl1 Sb1A 79.7(3) 18_654 3_665 ?
Sb1 Cl1 Sb1A 3.5(6) 16_544 3_665 ?
C2 C1 S1 116.8(6) . . ?
C2 C1 H1A 108.1 . . ?
S1 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
S1 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C3 C2 C3 118.3(6) 3_665 . ?
C3 C2 C1 119.4(7) 3_665 . ?
C3 C2 C1 122.3(7) . . ?
C2 C3 C2 121.7(6) 2_655 . ?
C2 C3 H3A 119.1 2_655 . ?
C2 C3 H3A 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sb1A Sb1 Sb1A Sb1 14(9) 18_654 . . 18_654 ?
S1 Sb1 Sb1A Sb1 142(5) 18_654 . . 18_654 ?
Cl1 Sb1 Sb1A Sb1 -44(29) . . . 18_654 ?
S1 Sb1 Sb1A Sb1 50(5) . . . 18_654 ?
Cl1 Sb1 Sb1A Sb1 -98(6) 16_544 . . 18_654 ?
Sb1 Sb1 Sb1A Sb1A -14(9) 18_654 . . 18_654 ?
S1 Sb1 Sb1A Sb1A 127(4) 18_654 . . 18_654 ?
Cl1 Sb1 Sb1A Sb1A -58(25) . . . 18_654 ?
S1 Sb1 Sb1A Sb1A 36(4) . . . 18_654 ?
Cl1 Sb1 Sb1A Sb1A -112(8) 16_544 . . 18_654 ?
Sb1A Sb1 Sb1A S1 -127(4) 18_654 . . 18_654 ?
Sb1 Sb1 Sb1A S1 -142(5) 18_654 . . 18_654 ?
Cl1 Sb1 Sb1A S1 175(100) . . . 18_654 ?
S1 Sb1 Sb1A S1 -91.21(9) . . . 18_654 ?
Cl1 Sb1 Sb1A S1 120(6) 16_544 . . 18_654 ?
Sb1A Sb1 Sb1A Cl1 80(10) 18_654 . . 18_654 ?
Sb1 Sb1 Sb1A Cl1 66(9) 18_654 . . 18_654 ?
S1 Sb1 Sb1A Cl1 -152(8) 18_654 . . 18_654 ?
Cl1 Sb1 Sb1A Cl1 22(34) . . . 18_654 ?
S1 Sb1 Sb1A Cl1 116(8) . . . 18_654 ?
Cl1 Sb1 Sb1A Cl1 -32(13) 16_544 . . 18_654 ?
Sb1A Sb1 Sb1A S1 -36(4) 18_654 . . . ?
Sb1 Sb1 Sb1A S1 -50(5) 18_654 . . . ?
S1 Sb1 Sb1A S1 91.21(9) 18_654 . . . ?
Cl1 Sb1 Sb1A S1 -94(27) . . . . ?
Cl1 Sb1 Sb1A S1 -149(6) 16_544 . . . ?
Sb1A Sb1 Sb1A Cl1 74(6) 18_654 . . 2_655 ?
Sb1 Sb1 Sb1A Cl1 59(5) 18_654 . . 2_655 ?
S1 Sb1 Sb1A Cl1 -159(3) 18_654 . . 2_655 ?
Cl1 Sb1 Sb1A Cl1 16(29) . . . 2_655 ?
S1 Sb1 Sb1A Cl1 110(3) . . . 2_655 ?
Cl1 Sb1 Sb1A Cl1 -39(8) 16_544 . . 2_655 ?
Sb1 Sb1A S1 C1 -39(10) 18_654 . . . ?
Sb1A Sb1A S1 C1 58.5(17) 18_654 . . . ?
Sb1 Sb1A S1 C1 67.7(11) . . . . ?
S1 Sb1A S1 C1 151.4(4) 18_654 . . . ?
Cl1 Sb1A S1 C1 -105.9(4) 18_654 . . . ?
Cl1 Sb1A S1 C1 -94.9(4) 2_655 . . . ?
Sb1 Sb1A S1 Sb1A -97(9) 18_654 . . 18_654 ?
Sb1 Sb1A S1 Sb1A 9.2(19) . . . 18_654 ?
S1 Sb1A S1 Sb1A 92.9(18) 18_654 . . 18_654 ?
Cl1 Sb1A S1 Sb1A -164.4(19) 18_654 . . 18_654 ?
Cl1 Sb1A S1 Sb1A -153.4(18) 2_655 . . 18_654 ?
Sb1A Sb1A S1 Sb1 97(9) 18_654 . . 18_654 ?
Sb1 Sb1A S1 Sb1 107(9) . . . 18_654 ?
S1 Sb1A S1 Sb1 -170(10) 18_654 . . 18_654 ?
Cl1 Sb1A S1 Sb1 -67(10) 18_654 . . 18_654 ?
Cl1 Sb1A S1 Sb1 -56(10) 2_655 . . 18_654 ?
Sb1 Sb1A S1 Sb1 -107(9) 18_654 . . . ?
Sb1A Sb1A S1 Sb1 -9.2(19) 18_654 . . . ?
S1 Sb1A S1 Sb1 83.7(11) 18_654 . . . ?
Cl1 Sb1A S1 Sb1 -173.6(12) 18_654 . . . ?
Cl1 Sb1A S1 Sb1 -162.5(12) 2_655 . . . ?
Sb1A Sb1 S1 C1 -28(14) 18_654 . . . ?
Sb1A Sb1 S1 C1 -115.0(11) . . . . ?
Sb1 Sb1 S1 C1 -104(2) 18_654 . . . ?
S1 Sb1 S1 C1 165.9(5) 18_654 . . . ?
Cl1 Sb1 S1 C1 61.5(5) . . . . ?
Cl1 Sb1 S1 C1 57.6(6) 16_544 . . . ?
Sb1A Sb1 S1 Sb1A -87(13) . . . 18_654 ?
Sb1 Sb1 S1 Sb1A -76(13) 18_654 . . 18_654 ?
S1 Sb1 S1 Sb1A -166(14) 18_654 . . 18_654 ?
Cl1 Sb1 S1 Sb1A 90(13) . . . 18_654 ?
Cl1 Sb1 S1 Sb1A 86(13) 16_544 . . 18_654 ?
Sb1A Sb1 S1 Sb1 76(13) 18_654 . . 18_654 ?
Sb1A Sb1 S1 Sb1 -11.1(19) . . . 18_654 ?
S1 Sb1 S1 Sb1 -90(2) 18_654 . . 18_654 ?
Cl1 Sb1 S1 Sb1 165(2) . . . 18_654 ?
Cl1 Sb1 S1 Sb1 162(2) 16_544 . . 18_654 ?
Sb1A Sb1 S1 Sb1A 87(13) 18_654 . . . ?
Sb1 Sb1 S1 Sb1A 11.1(19) 18_654 . . . ?
S1 Sb1 S1 Sb1A -79.1(12) 18_654 . . . ?
Cl1 Sb1 S1 Sb1A 176.6(13) . . . . ?
Cl1 Sb1 S1 Sb1A 172.7(13) 16_544 . . . ?
Sb1A Sb1 Cl1 Cl1 -126(5) 18_654 . . 16_544 ?
Sb1A Sb1 Cl1 Cl1 -68(27) . . . 16_544 ?
Sb1 Sb1 Cl1 Cl1 -104(4) 18_654 . . 16_544 ?
S1 Sb1 Cl1 Cl1 106.7(13) 18_654 . . 16_544 ?
S1 Sb1 Cl1 Cl1 -161.5(13) . . . 16_544 ?
Sb1A Sb1 Cl1 Sb1A 58(25) . . . 18_654 ?
Sb1 Sb1 Cl1 Sb1A 22(5) 18_654 . . 18_654 ?
S1 Sb1 Cl1 Sb1A -128(5) 18_654 . . 18_654 ?
S1 Sb1 Cl1 Sb1A -36(4) . . . 18_654 ?
Cl1 Sb1 Cl1 Sb1A 126(5) 16_544 . . 18_654 ?
Sb1A Sb1 Cl1 Sb1 -96(5) 18_654 . . 16_544 ?
Sb1A Sb1 Cl1 Sb1 -39(26) . . . 16_544 ?
Sb1 Sb1 Cl1 Sb1 -74(3) 18_654 . . 16_544 ?
S1 Sb1 Cl1 Sb1 135.8(10) 18_654 . . 16_544 ?
S1 Sb1 Cl1 Sb1 -132.4(8) . . . 16_544 ?
Cl1 Sb1 Cl1 Sb1 29.2(14) 16_544 . . 16_544 ?
Sb1A Sb1 Cl1 Sb1A -100(4) 18_654 . . 3_665 ?
Sb1A Sb1 Cl1 Sb1A -42(27) . . . 3_665 ?
Sb1 Sb1 Cl1 Sb1A -78(4) 18_654 . . 3_665 ?
S1 Sb1 Cl1 Sb1A 132.3(4) 18_654 . . 3_665 ?
S1 Sb1 Cl1 Sb1A -135.9(3) . . . 3_665 ?
Cl1 Sb1 Cl1 Sb1A 25.6(12) 16_544 . . 3_665 ?
Sb1A S1 C1 C2 37.5(7) 18_654 . . . ?
Sb1 S1 C1 C2 21.5(8) 18_654 . . . ?
Sb1A S1 C1 C2 23.7(8) . . . . ?
Sb1 S1 C1 C2 38.8(8) . . . . ?
S1 C1 C2 C3 -121.0(7) . . . 3_665 ?
S1 C1 C2 C3 60.2(8) . . . . ?
C3 C2 C3 C2 0.6(13) 3_665 . . 2_655 ?
C1 C2 C3 C2 179.4(5) . . . 2_655 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        65.82
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.160
####################################################################### 
# 
# 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_dwj105
_database_code_depnum_ccdc_archive 'CCDC 1041516'
_audit_update_record             
;
2014-12-30 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXLTL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H42 As3 Cl3 S6'
_chemical_formula_weight         998.17

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'
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'
As As 0.0499 2.0058 '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                   10.0055(19)
_cell_length_b                   12.424(2)
_cell_length_c                   16.522(3)
_cell_angle_alpha                81.285(3)
_cell_angle_beta                 88.456(3)
_cell_angle_gamma                84.579(3)
_cell_volume                     2020.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    5822
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.86

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3453
_exptl_absorpt_correction_T_max  0.8174
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      193(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19136
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0438
_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       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7061
_reflns_number_gt                5780
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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.

 In the crystal structure there are two C6H6 solvent molecules. 
 One of them is disordered and was treated  by SQUEEZE 
 [Van der Sluis,P. & Spek, A.L. (1990) Acta Cryst., Sect.A,A46,194-201.].  
 Corrections of the X-ray data by SQUEEZE is  104 electron; 
 the required values 84 electron for two C6H6 molecules in the full 
 unit cell. 


;

_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)+(0.1093P)²+27.6957P] 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         7061
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0909
_refine_ls_wR_factor_ref         0.2466
_refine_ls_wR_factor_gt          0.2390
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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
As1 As 0.74090(10) 0.66286(10) 0.87602(6) 0.0420(3) Uani 1 1 d . A 1
As2 As 0.71774(10) 0.54006(8) 0.65014(7) 0.0384(3) Uani 1 1 d . A 1
As3 As 0.75270(10) 0.90877(11) 0.66744(7) 0.0508(4) Uani 1 1 d . A 1
Cl1 Cl 0.7392(4) 0.4804(3) 0.9181(3) 0.0735(10) Uani 1 1 d . A 1
Cl2 Cl 0.7119(3) 0.5721(3) 0.5122(2) 0.0663(9) Uani 1 1 d . A 1
Cl3 Cl 0.7322(5) 1.0782(5) 0.7024(4) 0.131(2) Uani 1 1 d . A 1
S1 S 0.9017(3) 0.6977(3) 0.95361(19) 0.0628(9) Uani 1 1 d . A 1
S2 S 0.5946(3) 0.7231(3) 0.96469(19) 0.0572(8) Uani 1 1 d . A 1
S3 S 0.8705(3) 0.3992(2) 0.66924(19) 0.0442(6) Uani 1 1 d . A 1
S4 S 0.5614(3) 0.4258(2) 0.6758(2) 0.0565(8) Uani 1 1 d . A 1
S5 S 0.9036(3) 0.9348(3) 0.56917(18) 0.0521(8) Uani 1 1 d . A 1
S6 S 0.5994(3) 0.9332(3) 0.57366(18) 0.0590(9) Uani 1 1 d . A 1
C1 C 1.0566(11) 0.6527(9) 0.8995(6) 0.045(2) Uani 1 1 d . A 1
H1A H 1.1284 0.6973 0.9117 0.054 Uiso 1 1 calc R A 1
H1B H 1.0841 0.5759 0.9229 0.054 Uiso 1 1 calc R A 1
C2 C 1.0492(8) 0.6594(8) 0.8082(6) 0.0308(19) Uani 1 1 d . A 1
C3 C 1.0434(8) 0.5633(7) 0.7734(6) 0.031(2) Uani 1 1 d . A 1
C4 C 1.0361(8) 0.5698(7) 0.6894(6) 0.032(2) Uani 1 1 d . A 1
C5 C 1.0406(8) 0.6694(8) 0.6373(6) 0.033(2) Uani 1 1 d . A 1
C6 C 1.0484(8) 0.7645(7) 0.6727(6) 0.0279(19) Uani 1 1 d . A 1
C7 C 1.0500(8) 0.7610(7) 0.7574(6) 0.031(2) Uani 1 1 d . A 1
C8 C 1.0505(10) 0.4525(8) 0.8280(7) 0.046(3) Uani 1 1 d . A 1
H8A H 1.0454 0.3947 0.7942 0.068 Uiso 1 1 calc R A 1
H8B H 0.9753 0.4512 0.8673 0.068 Uiso 1 1 calc R A 1
H8C H 1.1354 0.4403 0.8577 0.068 Uiso 1 1 calc R A 1
C9 C 1.0276(10) 0.4654(8) 0.6535(7) 0.044(3) Uani 1 1 d . A 1
H9A H 1.1014 0.4118 0.6766 0.053 Uiso 1 1 calc R A 1
H9B H 1.0445 0.4817 0.5938 0.053 Uiso 1 1 calc R A 1
C10 C 1.0391(11) 0.6758(10) 0.5444(6) 0.047(3) Uani 1 1 d . A 1
H10A H 1.0338 0.6024 0.5304 0.071 Uiso 1 1 calc R A 1
H10B H 1.1214 0.7051 0.5208 0.071 Uiso 1 1 calc R A 1
H10C H 0.9610 0.7239 0.5225 0.071 Uiso 1 1 calc R A 1
C11 C 1.0595(10) 0.8722(8) 0.6192(7) 0.041(2) Uani 1 1 d . A 1
H11A H 1.1285 0.8618 0.5763 0.050 Uiso 1 1 calc R A 1
H11B H 1.0913 0.9239 0.6529 0.050 Uiso 1 1 calc R A 1
C12 C 1.0606(11) 0.8624(8) 0.7957(7) 0.046(2) Uani 1 1 d . A 1
H12A H 1.0604 0.9261 0.7528 0.069 Uiso 1 1 calc R A 1
H12B H 1.1443 0.8547 0.8264 0.069 Uiso 1 1 calc R A 1
H12C H 0.9841 0.8722 0.8330 0.069 Uiso 1 1 calc R A 1
C13 C 0.4308(11) 0.7123(10) 0.9175(7) 0.049(3) Uani 1 1 d . A 1
H13A H 0.3959 0.6431 0.9435 0.059 Uiso 1 1 calc R A 1
H13B H 0.3669 0.7730 0.9310 0.059 Uiso 1 1 calc R A 1
C14 C 0.4312(8) 0.7147(8) 0.8256(6) 0.032(2) Uani 1 1 d . A 1
C15 C 0.4219(9) 0.6200(8) 0.7939(7) 0.037(2) Uani 1 1 d . A 1
C16 C 0.4157(8) 0.6230(8) 0.7086(7) 0.040(2) Uani 1 1 d . A 1
C17 C 0.4208(8) 0.7211(8) 0.6555(6) 0.036(2) Uani 1 1 d . A 1
C18 C 0.4341(8) 0.8174(7) 0.6893(6) 0.0299(19) Uani 1 1 d . A 1
C19 C 0.4383(8) 0.8144(8) 0.7741(6) 0.0311(19) Uani 1 1 d . A 1
C20 C 0.4109(11) 0.5110(8) 0.8493(9) 0.055(3) Uani 1 1 d . A 1
H20A H 0.4161 0.5215 0.9067 0.083 Uiso 1 1 calc R A 1
H20B H 0.4847 0.4582 0.8366 0.083 Uiso 1 1 calc R A 1
H20C H 0.3249 0.4832 0.8401 0.083 Uiso 1 1 calc R A 1
C21 C 0.4044(10) 0.5179(9) 0.6730(9) 0.054(3) Uani 1 1 d . A 1
H21A H 0.3753 0.5375 0.6154 0.064 Uiso 1 1 calc R A 1
H21B H 0.3336 0.4776 0.7037 0.064 Uiso 1 1 calc R A 1
C22 C 0.4053(11) 0.7281(10) 0.5641(7) 0.048(3) Uani 1 1 d . A 1
H22A H 0.3975 0.6548 0.5506 0.072 Uiso 1 1 calc R A 1
H22B H 0.4841 0.7582 0.5359 0.072 Uiso 1 1 calc R A 1
H22C H 0.3244 0.7758 0.5466 0.072 Uiso 1 1 calc R A 1
C23 C 0.4398(10) 0.9243(9) 0.6335(7) 0.043(2) Uani 1 1 d . A 1
H23A H 0.4290 0.9846 0.6668 0.052 Uiso 1 1 calc R A 1
H23B H 0.3638 0.9343 0.5951 0.052 Uiso 1 1 calc R A 1
C24 C 0.4473(11) 0.9179(8) 0.8105(7) 0.043(2) Uani 1 1 d . A 1
H24A H 0.4499 0.9003 0.8704 0.064 Uiso 1 1 calc R A 1
H24B H 0.3687 0.9693 0.7946 0.064 Uiso 1 1 calc R A 1
H24C H 0.5291 0.9513 0.7904 0.064 Uiso 1 1 calc R A 1
C1S C 0.785(3) 0.8103(11) 0.2025(11) 0.104(7) Uani 1 1 d . B 1
H1SA H 0.7885 0.8074 0.1454 0.125 Uiso 1 1 calc R B 1
C2S C 0.6657(18) 0.7854(11) 0.2490(13) 0.086(5) Uani 1 1 d . B 1
H2SA H 0.5877 0.7681 0.2239 0.103 Uiso 1 1 calc R B 1
C3S C 0.6701(15) 0.7877(10) 0.3323(11) 0.073(4) Uani 1 1 d . B 1
H3SA H 0.5940 0.7683 0.3650 0.087 Uiso 1 1 calc R B 1
C4S C 0.7761(17) 0.8158(10) 0.3691(11) 0.077(4) Uani 1 1 d . B 1
H4SA H 0.7736 0.8181 0.4264 0.093 Uiso 1 1 calc R B 1
C5S C 0.8886(16) 0.8414(10) 0.3235(13) 0.080(5) Uani 1 1 d . B 1
H5SA H 0.9638 0.8611 0.3499 0.096 Uiso 1 1 calc R B 1
C6S C 0.8953(19) 0.8392(11) 0.2421(14) 0.085(5) Uani 1 1 d . B 1
H6SA H 0.9743 0.8571 0.2119 0.102 Uiso 1 1 calc R B 1


_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
As1 S1 2.198(3) . ?
As1 S2 2.205(3) . ?
As1 Cl1 2.269(4) . ?
As2 S4 2.201(3) . ?
As2 S3 2.203(3) . ?
As2 Cl2 2.255(4) . ?
As3 S6 2.178(3) . ?
As3 S5 2.196(3) . ?
As3 Cl3 2.255(5) . ?
S1 C1 1.850(12) . ?
S2 C13 1.859(11) . ?
S3 C9 1.836(10) . ?
S4 C21 1.851(10) . ?
S5 C11 1.834(9) . ?
S6 C23 1.859(11) . ?
C1 C2 1.502(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.407(13) . ?
C2 C3 1.408(13) . ?
C3 C4 1.382(14) . ?
C3 C8 1.525(13) . ?
C4 C5 1.400(13) . ?
C4 C9 1.515(13) . ?
C5 C6 1.404(13) . ?
C5 C10 1.525(14) . ?
C6 C7 1.394(13) . ?
C6 C11 1.499(13) . ?
C7 C12 1.506(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.515(15) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.371(14) . ?
C14 C19 1.399(13) . ?
C15 C16 1.407(16) . ?
C15 C20 1.527(13) . ?
C16 C17 1.395(15) . ?
C16 C21 1.526(14) . ?
C17 C18 1.413(13) . ?
C17 C22 1.510(15) . ?
C18 C19 1.397(13) . ?
C18 C23 1.502(14) . ?
C19 C24 1.512(14) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C1S C6S 1.40(3) . ?
C1S C2S 1.43(3) . ?
C1S H1SA 0.9500 . ?
C2S C3S 1.38(2) . ?
C2S H2SA 0.9500 . ?
C3S C4S 1.34(2) . ?
C3S H3SA 0.9500 . ?
C4S C5S 1.37(2) . ?
C4S H4SA 0.9500 . ?
C5S C6S 1.35(2) . ?
C5S H5SA 0.9500 . ?
C6S H6SA 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 As1 S2 88.16(13) . . ?
S1 As1 Cl1 99.54(15) . . ?
S2 As1 Cl1 99.13(14) . . ?
S4 As2 S3 88.78(10) . . ?
S4 As2 Cl2 100.20(15) . . ?
S3 As2 Cl2 100.53(12) . . ?
S6 As3 S5 88.23(12) . . ?
S6 As3 Cl3 98.6(2) . . ?
S5 As3 Cl3 98.45(17) . . ?
C1 S1 As1 103.3(4) . . ?
C13 S2 As1 102.8(4) . . ?
C9 S3 As2 102.2(4) . . ?
C21 S4 As2 103.1(4) . . ?
C11 S5 As3 102.8(4) . . ?
C23 S6 As3 103.6(3) . . ?
C2 C1 S1 116.9(7) . . ?
C2 C1 H1A 108.1 . . ?
S1 C1 H1A 108.1 . . ?
C2 C1 H1B 108.1 . . ?
S1 C1 H1B 108.1 . . ?
H1A C1 H1B 107.3 . . ?
C7 C2 C3 120.0(9) . . ?
C7 C2 C1 120.3(9) . . ?
C3 C2 C1 119.8(8) . . ?
C4 C3 C2 119.6(8) . . ?
C4 C3 C8 120.3(9) . . ?
C2 C3 C8 120.1(9) . . ?
C3 C4 C5 121.5(9) . . ?
C3 C4 C9 118.6(9) . . ?
C5 C4 C9 119.9(9) . . ?
C4 C5 C6 118.3(9) . . ?
C4 C5 C10 121.5(9) . . ?
C6 C5 C10 120.2(9) . . ?
C7 C6 C5 121.4(8) . . ?
C7 C6 C11 118.5(9) . . ?
C5 C6 C11 120.1(9) . . ?
C6 C7 C2 119.1(8) . . ?
C6 C7 C12 121.7(9) . . ?
C2 C7 C12 119.1(9) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 S3 117.7(7) . . ?
C4 C9 H9A 107.9 . . ?
S3 C9 H9A 107.9 . . ?
C4 C9 H9B 107.9 . . ?
S3 C9 H9B 107.9 . . ?
H9A C9 H9B 107.2 . . ?
C5 C10 H10A 109.5 . . ?
C5 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C5 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 S5 115.2(7) . . ?
C6 C11 H11A 108.5 . . ?
S5 C11 H11A 108.5 . . ?
C6 C11 H11B 108.5 . . ?
S5 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 S2 116.6(7) . . ?
C14 C13 H13A 108.1 . . ?
S2 C13 H13A 108.1 . . ?
C14 C13 H13B 108.1 . . ?
S2 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C19 120.8(9) . . ?
C15 C14 C13 119.7(9) . . ?
C19 C14 C13 119.4(9) . . ?
C14 C15 C16 119.8(8) . . ?
C14 C15 C20 121.5(10) . . ?
C16 C15 C20 118.6(10) . . ?
C17 C16 C15 120.9(9) . . ?
C17 C16 C21 119.1(11) . . ?
C15 C16 C21 120.1(10) . . ?
C16 C17 C18 118.4(9) . . ?
C16 C17 C22 122.0(9) . . ?
C18 C17 C22 119.5(9) . . ?
C19 C18 C17 120.6(9) . . ?
C19 C18 C23 119.8(9) . . ?
C17 C18 C23 119.6(9) . . ?
C18 C19 C14 119.5(9) . . ?
C18 C19 C24 120.7(8) . . ?
C14 C19 C24 119.8(9) . . ?
C15 C20 H20A 109.5 . . ?
C15 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C15 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 S4 114.6(7) . . ?
C16 C21 H21A 108.6 . . ?
S4 C21 H21A 108.6 . . ?
C16 C21 H21B 108.6 . . ?
S4 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 S6 113.1(7) . . ?
C18 C23 H23A 109.0 . . ?
S6 C23 H23A 109.0 . . ?
C18 C23 H23B 109.0 . . ?
S6 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C6S C1S C2S 119.4(16) . . ?
C6S C1S H1SA 120.3 . . ?
C2S C1S H1SA 120.3 . . ?
C3S C2S C1S 116.6(16) . . ?
C3S C2S H2SA 121.7 . . ?
C1S C2S H2SA 121.7 . . ?
C4S C3S C2S 123.3(16) . . ?
C4S C3S H3SA 118.4 . . ?
C2S C3S H3SA 118.4 . . ?
C3S C4S C5S 119.4(18) . . ?
C3S C4S H4SA 120.3 . . ?
C5S C4S H4SA 120.3 . . ?
C6S C5S C4S 121.8(17) . . ?
C6S C5S H5SA 119.1 . . ?
C4S C5S H5SA 119.1 . . ?
C5S C6S C1S 119.4(17) . . ?
C5S C6S H6SA 120.3 . . ?
C1S C6S H6SA 120.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 As1 S1 C1 178.6(4) . . . . ?
Cl1 As1 S1 C1 79.7(4) . . . . ?
S1 As1 S2 C13 177.9(4) . . . . ?
Cl1 As1 S2 C13 -82.7(4) . . . . ?
S4 As2 S3 C9 -179.2(4) . . . . ?
Cl2 As2 S3 C9 80.7(4) . . . . ?
S3 As2 S4 C21 176.0(5) . . . . ?
Cl2 As2 S4 C21 -83.5(5) . . . . ?
S6 As3 S5 C11 -159.9(4) . . . . ?
Cl3 As3 S5 C11 101.6(4) . . . . ?
S5 As3 S6 C23 -177.2(4) . . . . ?
Cl3 As3 S6 C23 -78.9(4) . . . . ?
As1 S1 C1 C2 29.2(9) . . . . ?
S1 C1 C2 C7 75.9(10) . . . . ?
S1 C1 C2 C3 -104.9(9) . . . . ?
C7 C2 C3 C4 -1.1(12) . . . . ?
C1 C2 C3 C4 179.7(8) . . . . ?
C7 C2 C3 C8 176.6(8) . . . . ?
C1 C2 C3 C8 -2.6(12) . . . . ?
C2 C3 C4 C5 3.0(12) . . . . ?
C8 C3 C4 C5 -174.7(8) . . . . ?
C2 C3 C4 C9 -179.0(8) . . . . ?
C8 C3 C4 C9 3.3(12) . . . . ?
C3 C4 C5 C6 -2.0(12) . . . . ?
C9 C4 C5 C6 180.0(8) . . . . ?
C3 C4 C5 C10 177.1(8) . . . . ?
C9 C4 C5 C10 -0.9(12) . . . . ?
C4 C5 C6 C7 -0.8(12) . . . . ?
C10 C5 C6 C7 -180.0(8) . . . . ?
C4 C5 C6 C11 177.3(8) . . . . ?
C10 C5 C6 C11 -1.8(12) . . . . ?
C5 C6 C7 C2 2.6(12) . . . . ?
C11 C6 C7 C2 -175.6(8) . . . . ?
C5 C6 C7 C12 179.0(8) . . . . ?
C11 C6 C7 C12 0.8(12) . . . . ?
C3 C2 C7 C6 -1.6(12) . . . . ?
C1 C2 C7 C6 177.5(8) . . . . ?
C3 C2 C7 C12 -178.1(8) . . . . ?
C1 C2 C7 C12 1.0(12) . . . . ?
C3 C4 C9 S3 70.8(11) . . . . ?
C5 C4 C9 S3 -111.1(9) . . . . ?
As2 S3 C9 C4 41.2(9) . . . . ?
C7 C6 C11 S5 -106.5(9) . . . . ?
C5 C6 C11 S5 75.3(10) . . . . ?
As3 S5 C11 C6 42.9(9) . . . . ?
As1 S2 C13 C14 -24.5(9) . . . . ?
S2 C13 C14 C15 105.0(9) . . . . ?
S2 C13 C14 C19 -76.4(11) . . . . ?
C19 C14 C15 C16 -1.7(13) . . . . ?
C13 C14 C15 C16 176.9(8) . . . . ?
C19 C14 C15 C20 -178.6(8) . . . . ?
C13 C14 C15 C20 0.0(13) . . . . ?
C14 C15 C16 C17 0.9(13) . . . . ?
C20 C15 C16 C17 177.9(8) . . . . ?
C14 C15 C16 C21 -179.6(8) . . . . ?
C20 C15 C16 C21 -2.6(13) . . . . ?
C15 C16 C17 C18 0.8(12) . . . . ?
C21 C16 C17 C18 -178.7(8) . . . . ?
C15 C16 C17 C22 -175.9(8) . . . . ?
C21 C16 C17 C22 4.5(13) . . . . ?
C16 C17 C18 C19 -1.7(12) . . . . ?
C22 C17 C18 C19 175.1(8) . . . . ?
C16 C17 C18 C23 -180.0(8) . . . . ?
C22 C17 C18 C23 -3.1(12) . . . . ?
C17 C18 C19 C14 1.0(12) . . . . ?
C23 C18 C19 C14 179.2(8) . . . . ?
C17 C18 C19 C24 -177.7(8) . . . . ?
C23 C18 C19 C24 0.5(12) . . . . ?
C15 C14 C19 C18 0.8(12) . . . . ?
C13 C14 C19 C18 -177.8(8) . . . . ?
C15 C14 C19 C24 179.5(8) . . . . ?
C13 C14 C19 C24 0.9(12) . . . . ?
C17 C16 C21 S4 105.1(10) . . . . ?
C15 C16 C21 S4 -74.4(11) . . . . ?
As2 S4 C21 C16 -37.1(10) . . . . ?
C19 C18 C23 S6 110.7(9) . . . . ?
C17 C18 C23 S6 -71.0(10) . . . . ?
As3 S6 C23 C18 -58.4(8) . . . . ?
C6S C1S C2S C3S -2(2) . . . . ?
C1S C2S C3S C4S 3(2) . . . . ?
C2S C3S C4S C5S -2(2) . . . . ?
C3S C4S C5S C6S 0(2) . . . . ?
C4S C5S C6S C1S 0(2) . . . . ?
C2S C1S C6S C5S 1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         3.694
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.185
####################################################################### 
# 
# 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_dwj112
_database_code_depnum_ccdc_archive 'CCDC 1041517'
_audit_update_record             
;
2014-12-30 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXTL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H42 As3 Cl3 S6'
_chemical_formula_weight         926.11

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'
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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.413(2)
_cell_length_b                   16.413(2)
_cell_length_c                   23.800(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5552.5(17)
_cell_formula_units_Z            6
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    2711
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      22.25

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2808
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_T_max  0.8280
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      193(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13363
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2175
_reflns_number_gt                1964
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1851P)²+9.1839P] 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         2175
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.2290
_refine_ls_wR_factor_gt          0.2213
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_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
As1 As 0.57691(5) 0.41037(6) 0.08700(3) 0.0338(4) Uani 1 1 d . . .
Cl1 Cl 0.65849(15) 0.56952(16) 0.08847(9) 0.0580(7) Uani 1 1 d . . .
S1 S 0.46689(11) 0.38091(12) 0.02347(8) 0.0292(5) Uani 1 1 d . . .
S2 S 0.46601(12) 0.38025(14) 0.15018(8) 0.0371(5) Uani 1 1 d . . .
C1 C 0.5237(5) 0.3876(4) -0.0445(3) 0.0264(14) Uani 1 1 d . . .
H1A H 0.4745 0.3467 -0.0716 0.032 Uiso 1 1 calc R . .
H1B H 0.5525 0.4530 -0.0586 0.032 Uiso 1 1 calc R . .
C2 C 0.5976(4) 0.3598(4) -0.0432(2) 0.0200(13) Uani 1 1 d . . .
C3 C 0.5702(4) 0.2634(4) -0.0429(3) 0.0233(14) Uani 1 1 d . . .
C4 C 0.4681(4) 0.1894(4) -0.0485(3) 0.0280(15) Uani 1 1 d . . .
H4A H 0.4287 0.2126 -0.0311 0.034 Uiso 1 1 calc R . .
H4B H 0.4565 0.1321 -0.0280 0.034 Uiso 1 1 calc R . .
C5 C 0.4390(5) 0.1641(5) -0.1102(3) 0.0399(18) Uani 1 1 d . . .
H5A H 0.3723 0.1160 -0.1122 0.060 Uiso 1 1 calc R . .
H5B H 0.4769 0.1398 -0.1274 0.060 Uiso 1 1 calc R . .
H5C H 0.4493 0.2204 -0.1306 0.060 Uiso 1 1 calc R . .
C6 C 0.5241(5) 0.3886(5) 0.2178(3) 0.0282(15) Uani 1 1 d . . .
H6A H 0.5534 0.4544 0.2312 0.034 Uiso 1 1 calc R . .
H6B H 0.4752 0.3488 0.2455 0.034 Uiso 1 1 calc R . .
C7 C 0.5984(4) 0.3601(4) 0.2176(3) 0.0232(13) Uani 1 1 d . . .
C8 C 0.6940(4) 0.4294(4) 0.2169(2) 0.0224(13) Uani 1 1 d . . .
C9 C 0.7237(5) 0.5337(5) 0.2217(3) 0.0317(16) Uani 1 1 d . . .
H9A H 0.7849 0.5718 0.2025 0.038 Uiso 1 1 calc R . .
H9B H 0.6767 0.5447 0.2024 0.038 Uiso 1 1 calc R . .
C10 C 0.7327(6) 0.5658(6) 0.2824(3) 0.0461(19) Uani 1 1 d . . .
H10A H 0.7517 0.6327 0.2834 0.069 Uiso 1 1 calc R . .
H10B H 0.7801 0.5562 0.3015 0.069 Uiso 1 1 calc R . .
H10C H 0.6719 0.5291 0.3014 0.069 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
As1 S1 2.2153(18) . ?
As1 S2 2.2177(19) . ?
As1 Cl1 2.263(2) . ?
S1 C1 1.842(7) . ?
S2 C6 1.841(7) . ?
C1 C2 1.496(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.407(8) 3_665 ?
C2 C3 1.412(8) . ?
C3 C2 1.407(8) 2_655 ?
C3 C4 1.506(8) . ?
C4 C5 1.536(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.508(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.397(9) 2_655 ?
C7 C8 1.404(8) . ?
C8 C7 1.397(9) 3_665 ?
C8 C9 1.531(8) . ?
C9 C10 1.519(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 As1 S2 85.73(7) . . ?
S1 As1 Cl1 102.11(7) . . ?
S2 As1 Cl1 101.12(9) . . ?
C1 S1 As1 104.7(2) . . ?
C6 S2 As1 103.8(2) . . ?
C2 C1 S1 115.3(5) . . ?
C2 C1 H1A 108.4 . . ?
S1 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
S1 C1 H1B 108.4 . . ?
H1A C1 H1B 107.5 . . ?
C3 C2 C3 121.1(6) 3_665 . ?
C3 C2 C1 119.6(5) 3_665 . ?
C3 C2 C1 119.3(5) . . ?
C2 C3 C2 118.9(6) 2_655 . ?
C2 C3 C4 120.3(5) 2_655 . ?
C2 C3 C4 120.4(5) . . ?
C3 C4 C5 111.9(6) . . ?
C3 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 S2 116.3(5) . . ?
C7 C6 H6A 108.2 . . ?
S2 C6 H6A 108.2 . . ?
C7 C6 H6B 108.2 . . ?
S2 C6 H6B 108.2 . . ?
H6A C6 H6B 107.4 . . ?
C8 C7 C8 121.0(6) 2_655 . ?
C8 C7 C6 119.1(5) 2_655 . ?
C8 C7 C6 119.9(5) . . ?
C7 C8 C7 119.0(6) 3_665 . ?
C7 C8 C9 120.3(5) 3_665 . ?
C7 C8 C9 120.5(6) . . ?
C10 C9 C8 112.3(6) . . ?
C10 C9 H9A 109.1 . . ?
C8 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 As1 S1 C1 -175.5(2) . . . . ?
Cl1 As1 S1 C1 84.0(2) . . . . ?
S1 As1 S2 C6 176.4(2) . . . . ?
Cl1 As1 S2 C6 -82.1(2) . . . . ?
As1 S1 C1 C2 30.6(5) . . . . ?
S1 C1 C2 C3 -101.6(6) . . . 3_665 ?
S1 C1 C2 C3 79.1(7) . . . . ?
C3 C2 C3 C2 -1.0(12) 3_665 . . 2_655 ?
C1 C2 C3 C2 178.3(4) . . . 2_655 ?
C3 C2 C3 C4 -174.4(4) 3_665 . . . ?
C1 C2 C3 C4 4.9(9) . . . . ?
C2 C3 C4 C5 -84.0(7) 2_655 . . . ?
C2 C3 C4 C5 89.3(7) . . . . ?
As1 S2 C6 C7 -31.8(5) . . . . ?
S2 C6 C7 C8 -77.0(7) . . . 2_655 ?
S2 C6 C7 C8 101.6(6) . . . . ?
C8 C7 C8 C7 -2.4(13) 2_655 . . 3_665 ?
C6 C7 C8 C7 179.0(4) . . . 3_665 ?
C8 C7 C8 C9 -175.8(4) 2_655 . . . ?
C6 C7 C8 C9 5.5(9) . . . . ?
C7 C8 C9 C10 -86.8(8) 3_665 . . . ?
C7 C8 C9 C10 86.6(8) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.161
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.144
####################################################################### 
# 
# 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_dwj115
_database_code_depnum_ccdc_archive 'CCDC 1041518'
_audit_update_record             
;
2014-12-30 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXTL
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H30 Cl3 S6 Sb3'
_chemical_formula_weight         982.44

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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   16.0971(10)
_cell_length_b                   11.4604(7)
_cell_length_c                   16.3368(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.8670(10)
_cell_angle_gamma                90.00
_cell_volume                     3012.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9982
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1896
_exptl_absorpt_coefficient_mu    3.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_T_max  0.9056
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26103
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6582
_reflns_number_gt                5889
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0237P)²+6.1073P] 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         6582
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0577
_refine_ls_wR_factor_gt          0.0553
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_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
Sb1 Sb 0.280412(12) 0.905478(18) -0.081689(13) 0.01254(6) Uani 1 1 d . . .
Sb2 Sb 0.348239(12) 0.668762(18) 0.066191(13) 0.01118(5) Uani 1 1 d . . .
Sb3 Sb 0.121942(11) 0.726240(18) 0.032265(13) 0.01131(5) Uani 1 1 d . . .
Cl1 Cl 0.14172(6) 0.96429(9) -0.12495(6) 0.0338(2) Uani 1 1 d . . .
Cl2 Cl 0.46052(5) 0.76692(7) -0.00112(5) 0.01945(17) Uani 1 1 d . . .
Cl3 Cl 0.15019(5) 0.56577(7) 0.12658(5) 0.02011(17) Uani 1 1 d . . .
S1 S 0.34015(6) 1.09573(7) -0.06316(5) 0.01957(17) Uani 1 1 d . . .
S2 S 0.40735(5) 0.66747(7) 0.20311(5) 0.01712(17) Uani 1 1 d . . .
S3 S 0.01716(5) 0.82143(7) 0.10832(5) 0.01750(17) Uani 1 1 d . . .
S4 S 0.34275(6) 0.89719(7) -0.21250(5) 0.02112(18) Uani 1 1 d . . .
S5 S 0.39442(5) 0.47097(7) 0.05155(5) 0.01351(15) Uani 1 1 d . . .
S6 S 0.01276(4) 0.64318(7) -0.05216(5) 0.01344(16) Uani 1 1 d . . .
C1 C 0.28465(19) 1.0339(3) 0.09591(18) 0.0117(6) Uani 1 1 d . . .
C2 C 0.34252(18) 0.9646(3) 0.14078(19) 0.0116(6) Uani 1 1 d . . .
C3 C 0.31323(18) 0.8790(3) 0.19387(19) 0.0122(6) Uani 1 1 d . . .
C4 C 0.22754(19) 0.8626(3) 0.20378(18) 0.0119(6) Uani 1 1 d . . .
C5 C 0.17057(18) 0.9326(3) 0.15897(18) 0.0112(6) Uani 1 1 d . . .
C6 C 0.19875(18) 1.0180(3) 0.10432(18) 0.0111(6) Uani 1 1 d . . .
C7 C 0.3159(2) 1.1323(3) 0.0440(2) 0.0152(6) Uani 1 1 d . . .
H7A H 0.3668 1.1644 0.0712 0.018 Uiso 1 1 calc R . .
H7B H 0.2736 1.1950 0.0428 0.018 Uiso 1 1 calc R . .
C8 C 0.43471(19) 0.9877(3) 0.1343(2) 0.0184(7) Uani 1 1 d . . .
H8A H 0.4660 0.9323 0.1690 0.028 Uiso 1 1 calc R . .
H8B H 0.4472 1.0675 0.1525 0.028 Uiso 1 1 calc R . .
H8C H 0.4506 0.9783 0.0773 0.028 Uiso 1 1 calc R . .
C9 C 0.3749(2) 0.8095(3) 0.2458(2) 0.0169(7) Uani 1 1 d . . .
H9A H 0.3503 0.7951 0.2996 0.020 Uiso 1 1 calc R . .
H9B H 0.4252 0.8579 0.2555 0.020 Uiso 1 1 calc R . .
C10 C 0.1979(2) 0.7759(3) 0.2664(2) 0.0190(7) Uani 1 1 d . . .
H10A H 0.1370 0.7751 0.2654 0.028 Uiso 1 1 calc R . .
H10B H 0.2190 0.7987 0.3210 0.028 Uiso 1 1 calc R . .
H10C H 0.2185 0.6979 0.2532 0.028 Uiso 1 1 calc R . .
C11 C 0.07885(19) 0.9233(3) 0.1742(2) 0.0165(7) Uani 1 1 d . . .
H11A H 0.0542 1.0021 0.1679 0.020 Uiso 1 1 calc R . .
H11B H 0.0725 0.8994 0.2319 0.020 Uiso 1 1 calc R . .
C12 C 0.1366(2) 1.0945(3) 0.0593(2) 0.0188(7) Uani 1 1 d . . .
H12A H 0.1658 1.1489 0.0240 0.028 Uiso 1 1 calc R . .
H12B H 0.1046 1.1386 0.0989 0.028 Uiso 1 1 calc R . .
H12C H 0.0988 1.0459 0.0257 0.028 Uiso 1 1 calc R . .
C13 C 0.27036(18) 0.6730(3) -0.19548(18) 0.0100(6) Uani 1 1 d . . .
C14 C 0.33072(17) 0.6026(3) -0.15514(18) 0.0100(6) Uani 1 1 d . . .
C15 C 0.30608(17) 0.5175(3) -0.09957(18) 0.0095(6) Uani 1 1 d . . .
C16 C 0.22066(17) 0.4989(3) -0.08553(18) 0.0093(6) Uani 1 1 d . . .
C17 C 0.16133(17) 0.5686(3) -0.12671(18) 0.0104(6) Uani 1 1 d . . .
C18 C 0.18544(18) 0.6565(3) -0.18189(18) 0.0105(6) Uani 1 1 d . . .
C19 C 0.29784(18) 0.7617(3) -0.25734(18) 0.0124(6) Uani 1 1 d . . .
H19A H 0.2494 0.7828 -0.2932 0.015 Uiso 1 1 calc R . .
H19B H 0.3397 0.7250 -0.2922 0.015 Uiso 1 1 calc R . .
C20 C 0.42087(18) 0.6143(3) -0.1770(2) 0.0148(6) Uani 1 1 d . . .
H20A H 0.4547 0.5599 -0.1437 0.022 Uiso 1 1 calc R . .
H20B H 0.4396 0.6943 -0.1662 0.022 Uiso 1 1 calc R . .
H20C H 0.4267 0.5962 -0.2351 0.022 Uiso 1 1 calc R . .
C21 C 0.36970(18) 0.4388(3) -0.05794(19) 0.0127(6) Uani 1 1 d . . .
H21A H 0.4218 0.4435 -0.0884 0.015 Uiso 1 1 calc R . .
H21B H 0.3494 0.3574 -0.0622 0.015 Uiso 1 1 calc R . .
C22 C 0.19625(18) 0.3980(3) -0.03244(19) 0.0126(6) Uani 1 1 d . . .
H22A H 0.1357 0.3963 -0.0284 0.019 Uiso 1 1 calc R . .
H22B H 0.2221 0.4071 0.0223 0.019 Uiso 1 1 calc R . .
H22C H 0.2151 0.3249 -0.0568 0.019 Uiso 1 1 calc R . .
C23 C 0.06980(17) 0.5429(3) -0.11886(19) 0.0110(6) Uani 1 1 d . . .
H23A H 0.0640 0.4626 -0.0975 0.013 Uiso 1 1 calc R . .
H23B H 0.0430 0.5448 -0.1742 0.013 Uiso 1 1 calc R . .
C24 C 0.11849(18) 0.7207(3) -0.23035(19) 0.0138(6) Uani 1 1 d . . .
H24A H 0.1441 0.7787 -0.2657 0.021 Uiso 1 1 calc R . .
H24B H 0.0815 0.7601 -0.1927 0.021 Uiso 1 1 calc R . .
H24C H 0.0864 0.6650 -0.2641 0.021 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
Sb1 S4 2.3923(9) . ?
Sb1 S1 2.3982(8) . ?
Sb1 Cl1 2.4156(9) . ?
Sb2 S5 2.3999(8) . ?
Sb2 S2 2.4022(8) . ?
Sb2 Cl2 2.4230(8) . ?
Sb3 S3 2.3907(8) . ?
Sb3 S6 2.3957(8) . ?
Sb3 Cl3 2.4326(8) . ?
S1 C7 1.854(3) . ?
S2 C9 1.853(3) . ?
S3 C11 1.854(3) . ?
S4 C19 1.854(3) . ?
S5 C21 1.857(3) . ?
S6 C23 1.849(3) . ?
C1 C6 1.406(4) . ?
C1 C2 1.411(4) . ?
C1 C7 1.507(4) . ?
C2 C3 1.401(4) . ?
C2 C8 1.514(4) . ?
C3 C4 1.407(4) . ?
C3 C9 1.511(4) . ?
C4 C5 1.406(4) . ?
C4 C10 1.513(4) . ?
C5 C6 1.410(4) . ?
C5 C11 1.509(4) . ?
C6 C12 1.505(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.405(4) . ?
C13 C14 1.410(4) . ?
C13 C19 1.510(4) . ?
C14 C15 1.399(4) . ?
C14 C20 1.511(4) . ?
C15 C16 1.418(4) . ?
C15 C21 1.510(4) . ?
C16 C17 1.400(4) . ?
C16 C22 1.506(4) . ?
C17 C18 1.415(4) . ?
C17 C23 1.512(4) . ?
C18 C24 1.508(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Sb1 S1 88.32(3) . . ?
S4 Sb1 Cl1 99.22(4) . . ?
S1 Sb1 Cl1 98.41(3) . . ?
S5 Sb2 S2 88.42(3) . . ?
S5 Sb2 Cl2 98.93(3) . . ?
S2 Sb2 Cl2 98.44(3) . . ?
S3 Sb3 S6 87.92(3) . . ?
S3 Sb3 Cl3 97.83(3) . . ?
S6 Sb3 Cl3 100.53(3) . . ?
C7 S1 Sb1 103.23(10) . . ?
C9 S2 Sb2 103.70(10) . . ?
C11 S3 Sb3 102.44(10) . . ?
C19 S4 Sb1 102.52(10) . . ?
C21 S5 Sb2 103.08(10) . . ?
C23 S6 Sb3 102.55(9) . . ?
C6 C1 C2 120.7(3) . . ?
C6 C1 C7 120.0(3) . . ?
C2 C1 C7 119.1(3) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 C8 121.0(3) . . ?
C1 C2 C8 119.8(3) . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 C9 119.2(3) . . ?
C4 C3 C9 119.5(3) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 C10 120.8(3) . . ?
C3 C4 C10 119.8(3) . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 C11 119.9(3) . . ?
C6 C5 C11 119.3(3) . . ?
C1 C6 C5 119.3(3) . . ?
C1 C6 C12 121.2(3) . . ?
C5 C6 C12 119.4(3) . . ?
C1 C7 S1 116.5(2) . . ?
C1 C7 H7A 108.2 . . ?
S1 C7 H7A 108.2 . . ?
C1 C7 H7B 108.2 . . ?
S1 C7 H7B 108.2 . . ?
H7A C7 H7B 107.3 . . ?
C2 C8 H8A 109.5 . . ?
C2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C9 S2 116.1(2) . . ?
C3 C9 H9A 108.3 . . ?
S2 C9 H9A 108.3 . . ?
C3 C9 H9B 108.3 . . ?
S2 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C11 S3 117.2(2) . . ?
C5 C11 H11A 108.0 . . ?
S3 C11 H11A 108.0 . . ?
C5 C11 H11B 108.0 . . ?
S3 C11 H11B 108.0 . . ?
H11A C11 H11B 107.2 . . ?
C6 C12 H12A 109.5 . . ?
C6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 120.6(3) . . ?
C18 C13 C19 120.3(3) . . ?
C14 C13 C19 119.1(3) . . ?
C15 C14 C13 119.8(3) . . ?
C15 C14 C20 120.6(3) . . ?
C13 C14 C20 119.4(3) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 C21 120.4(3) . . ?
C16 C15 C21 119.0(3) . . ?
C17 C16 C15 119.1(3) . . ?
C17 C16 C22 121.9(3) . . ?
C15 C16 C22 118.8(3) . . ?
C16 C17 C18 121.0(3) . . ?
C16 C17 C23 120.0(3) . . ?
C18 C17 C23 118.8(3) . . ?
C13 C18 C17 119.0(3) . . ?
C13 C18 C24 122.3(3) . . ?
C17 C18 C24 118.4(3) . . ?
C13 C19 S4 114.7(2) . . ?
C13 C19 H19A 108.6 . . ?
S4 C19 H19A 108.6 . . ?
C13 C19 H19B 108.6 . . ?
S4 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C14 C20 H20A 109.5 . . ?
C14 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C14 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C15 C21 S5 115.8(2) . . ?
C15 C21 H21A 108.3 . . ?
S5 C21 H21A 108.3 . . ?
C15 C21 H21B 108.3 . . ?
S5 C21 H21B 108.3 . . ?
H21A C21 H21B 107.4 . . ?
C16 C22 H22A 109.5 . . ?
C16 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C16 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C17 C23 S6 115.7(2) . . ?
C17 C23 H23A 108.4 . . ?
S6 C23 H23A 108.4 . . ?
C17 C23 H23B 108.4 . . ?
S6 C23 H23B 108.4 . . ?
H23A C23 H23B 107.4 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S4 Sb1 S1 C7 -173.38(11) . . . . ?
Cl1 Sb1 S1 C7 87.55(11) . . . . ?
S5 Sb2 S2 C9 -174.07(12) . . . . ?
Cl2 Sb2 S2 C9 87.13(12) . . . . ?
S6 Sb3 S3 C11 -170.05(12) . . . . ?
Cl3 Sb3 S3 C11 89.60(12) . . . . ?
S1 Sb1 S4 C19 -172.50(10) . . . . ?
Cl1 Sb1 S4 C19 -74.26(10) . . . . ?
S2 Sb2 S5 C21 -173.83(10) . . . . ?
Cl2 Sb2 S5 C21 -75.53(10) . . . . ?
S3 Sb3 S6 C23 -174.17(11) . . . . ?
Cl3 Sb3 S6 C23 -76.59(11) . . . . ?
C6 C1 C2 C3 0.2(4) . . . . ?
C7 C1 C2 C3 175.1(3) . . . . ?
C6 C1 C2 C8 -176.6(3) . . . . ?
C7 C1 C2 C8 -1.7(4) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C8 C2 C3 C4 175.9(3) . . . . ?
C1 C2 C3 C9 -176.4(3) . . . . ?
C8 C2 C3 C9 0.4(4) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C9 C3 C4 C5 176.1(3) . . . . ?
C2 C3 C4 C10 -175.3(3) . . . . ?
C9 C3 C4 C10 0.2(4) . . . . ?
C3 C4 C5 C6 0.3(4) . . . . ?
C10 C4 C5 C6 176.2(3) . . . . ?
C3 C4 C5 C11 -174.7(3) . . . . ?
C10 C4 C5 C11 1.1(4) . . . . ?
C2 C1 C6 C5 0.7(4) . . . . ?
C7 C1 C6 C5 -174.2(3) . . . . ?
C2 C1 C6 C12 177.6(3) . . . . ?
C7 C1 C6 C12 2.7(4) . . . . ?
C4 C5 C6 C1 -1.0(4) . . . . ?
C11 C5 C6 C1 174.1(3) . . . . ?
C4 C5 C6 C12 -177.9(3) . . . . ?
C11 C5 C6 C12 -2.8(4) . . . . ?
C6 C1 C7 S1 -95.8(3) . . . . ?
C2 C1 C7 S1 89.3(3) . . . . ?
Sb1 S1 C7 C1 12.2(3) . . . . ?
C2 C3 C9 S2 -94.5(3) . . . . ?
C4 C3 C9 S2 89.9(3) . . . . ?
Sb2 S2 C9 C3 8.4(3) . . . . ?
C4 C5 C11 S3 -93.2(3) . . . . ?
C6 C5 C11 S3 91.7(3) . . . . ?
Sb3 S3 C11 C5 6.7(3) . . . . ?
C18 C13 C14 C15 -1.6(4) . . . . ?
C19 C13 C14 C15 -178.0(3) . . . . ?
C18 C13 C14 C20 174.1(3) . . . . ?
C19 C13 C14 C20 -2.3(4) . . . . ?
C13 C14 C15 C16 2.1(4) . . . . ?
C20 C14 C15 C16 -173.6(3) . . . . ?
C13 C14 C15 C21 178.0(3) . . . . ?
C20 C14 C15 C21 2.3(4) . . . . ?
C14 C15 C16 C17 -1.4(4) . . . . ?
C21 C15 C16 C17 -177.3(3) . . . . ?
C14 C15 C16 C22 173.4(3) . . . . ?
C21 C15 C16 C22 -2.6(4) . . . . ?
C15 C16 C17 C18 0.1(4) . . . . ?
C22 C16 C17 C18 -174.4(3) . . . . ?
C15 C16 C17 C23 174.2(3) . . . . ?
C22 C16 C17 C23 -0.3(4) . . . . ?
C14 C13 C18 C17 0.4(4) . . . . ?
C19 C13 C18 C17 176.7(3) . . . . ?
C14 C13 C18 C24 -173.2(3) . . . . ?
C19 C13 C18 C24 3.1(4) . . . . ?
C16 C17 C18 C13 0.4(4) . . . . ?
C23 C17 C18 C13 -173.8(3) . . . . ?
C16 C17 C18 C24 174.2(3) . . . . ?
C23 C17 C18 C24 0.1(4) . . . . ?
C18 C13 C19 S4 105.4(3) . . . . ?
C14 C13 C19 S4 -78.2(3) . . . . ?
Sb1 S4 C19 C13 -25.2(2) . . . . ?
C14 C15 C21 S5 105.7(3) . . . . ?
C16 C15 C21 S5 -78.4(3) . . . . ?
Sb2 S5 C21 C15 -19.6(2) . . . . ?
C16 C17 C23 S6 104.8(3) . . . . ?
C18 C17 C23 S6 -81.0(3) . . . . ?
Sb3 S6 C23 C17 -21.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.114
####################################################################### 
# 
# 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_mo_asr121_0m
_database_code_depnum_ccdc_archive 'CCDC 1041519'
_audit_update_record             
;
2014-12-30 deposited with the CCDC.
2015-02-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXTL
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H42 Cl3 S6 Sb3'
_chemical_formula_weight         1066.60

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'
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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   16.4580(6)
_cell_length_b                   16.4580(6)
_cell_length_c                   23.9449(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5616.9(3)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      3.88
_cell_measurement_theta_max      39.34

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3132
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7020
_exptl_absorpt_correction_T_max  0.8990
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Triumph mirror'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14133
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         28.00
_reflns_number_total             3020
_reflns_number_gt                2720
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0349P)²+14.1265P] 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         3020
_refine_ls_number_parameters     127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0250
_refine_ls_wR_factor_ref         0.0706
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_restrained_S_all      1.162
_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
Sb1 Sb 0.759127(13) 0.263363(12) 0.078952(8) 0.01608(8) Uani 1 1 d . . .
S1 S 0.71674(5) 0.13826(5) 0.14468(3) 0.01730(14) Uani 1 1 d . . .
S2 S 0.71831(5) 0.13843(5) 0.01310(3) 0.02017(15) Uani 1 1 d . . .
Cl1 Cl 0.92797(5) 0.33509(5) 0.07814(3) 0.02412(16) Uani 1 1 d . . .
C1 C 0.72019(19) 0.18941(19) 0.21397(11) 0.0161(5) Uani 1 1 d . . .
H1A H 0.6776 0.1385 0.2395 0.019 Uiso 1 1 calc R . .
H1B H 0.7846 0.2170 0.2292 0.019 Uiso 1 1 calc R . .
C2 C 0.69245(19) 0.26373(19) 0.21310(10) 0.0134(5) Uani 1 1 d . . .
C3 C 0.59646(19) 0.23751(18) 0.21281(11) 0.0140(5) Uani 1 1 d . . .
C4 C 0.52119(19) 0.13479(19) 0.21607(12) 0.0179(5) Uani 1 1 d . . .
H4A H 0.5446 0.0961 0.1983 0.021 Uiso 1 1 calc R . .
H4B H 0.4651 0.1250 0.1952 0.021 Uiso 1 1 calc R . .
C5 C 0.4935(2) 0.1027(2) 0.27692(13) 0.0226(6) Uani 1 1 d . . .
H5A H 0.4448 0.0363 0.2775 0.034 Uiso 1 1 calc R . .
H5B H 0.4693 0.1402 0.2945 0.034 Uiso 1 1 calc R . .
H5C H 0.5486 0.1111 0.2975 0.034 Uiso 1 1 calc R . .
C6 C 0.7223(2) 0.1909(2) -0.05581(11) 0.0167(5) Uani 1 1 d . . .
H6A H 0.7869 0.2191 -0.0707 0.020 Uiso 1 1 calc R . .
H6B H 0.6804 0.1403 -0.0817 0.020 Uiso 1 1 calc R . .
C7 C 0.69388(19) 0.26500(19) -0.05495(11) 0.0140(5) Uani 1 1 d . . .
C8 C 0.59712(19) 0.23681(19) -0.05468(10) 0.0144(5) Uani 1 1 d . . .
C9 C 0.52409(19) 0.13334(19) -0.05696(12) 0.0179(5) Uani 1 1 d . . .
H9A H 0.4672 0.1230 -0.0368 0.021 Uiso 1 1 calc R . .
H9B H 0.5488 0.0971 -0.0375 0.021 Uiso 1 1 calc R . .
C10 C 0.4974(2) 0.0967(2) -0.11626(13) 0.0242(6) Uani 1 1 d . . .
H10A H 0.4501 0.0298 -0.1153 0.036 Uiso 1 1 calc R . .
H10B H 0.5532 0.1052 -0.1362 0.036 Uiso 1 1 calc R . .
H10C H 0.4717 0.1314 -0.1356 0.036 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
Sb1 S1 2.4014(7) . ?
Sb1 S2 2.4050(7) . ?
Sb1 Cl1 2.4156(7) . ?
S1 C1 1.848(3) . ?
S2 C6 1.848(3) . ?
C1 C2 1.505(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.407(4) 2_655 ?
C2 C3 1.414(4) . ?
C3 C2 1.407(4) 3_665 ?
C3 C4 1.518(4) . ?
C4 C5 1.539(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.510(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.404(4) 2_655 ?
C7 C8 1.419(4) . ?
C8 C7 1.404(4) 3_665 ?
C8 C9 1.517(4) . ?
C9 C10 1.519(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Sb1 S2 81.92(2) . . ?
S1 Sb1 Cl1 101.20(2) . . ?
S2 Sb1 Cl1 100.01(3) . . ?
C1 S1 Sb1 105.56(9) . . ?
C6 S2 Sb1 104.86(9) . . ?
C2 C1 S1 113.89(18) . . ?
C2 C1 H1A 108.8 . . ?
S1 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
S1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C3 120.5(3) 2_655 . ?
C3 C2 C1 119.5(2) 2_655 . ?
C3 C2 C1 119.9(2) . . ?
C2 C3 C2 119.5(3) 3_665 . ?
C2 C3 C4 120.1(2) 3_665 . ?
C2 C3 C4 120.3(2) . . ?
C3 C4 C5 111.6(2) . . ?
C3 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 S2 114.35(18) . . ?
C7 C6 H6A 108.7 . . ?
S2 C6 H6A 108.7 . . ?
C7 C6 H6B 108.7 . . ?
S2 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C8 C7 C8 121.1(3) 2_655 . ?
C8 C7 C6 119.7(2) 2_655 . ?
C8 C7 C6 119.1(2) . . ?
C7 C8 C7 118.8(3) 3_665 . ?
C7 C8 C9 121.3(2) 3_665 . ?
C7 C8 C9 119.8(2) . . ?
C8 C9 C10 112.9(2) . . ?
C8 C9 H9A 109.0 . . ?
C10 C9 H9A 109.0 . . ?
C8 C9 H9B 109.0 . . ?
C10 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S2 Sb1 S1 C1 -173.35(9) . . . . ?
Cl1 Sb1 S1 C1 87.98(9) . . . . ?
S1 Sb1 S2 C6 172.60(10) . . . . ?
Cl1 Sb1 S2 C6 -87.36(10) . . . . ?
Sb1 S1 C1 C2 33.0(2) . . . . ?
S1 C1 C2 C3 -99.0(3) . . . 2_655 ?
S1 C1 C2 C3 81.2(3) . . . . ?
C3 C2 C3 C2 -0.9(5) 2_655 . . 3_665 ?
C1 C2 C3 C2 178.77(17) . . . 3_665 ?
C3 C2 C3 C4 -176.90(18) 2_655 . . . ?
C1 C2 C3 C4 2.8(4) . . . . ?
C2 C3 C4 C5 -85.3(3) 3_665 . . . ?
C2 C3 C4 C5 90.6(3) . . . . ?
Sb1 S2 C6 C7 -33.0(2) . . . . ?
S2 C6 C7 C8 99.6(3) . . . 2_655 ?
S2 C6 C7 C8 -80.6(3) . . . . ?
C8 C7 C8 C7 0.9(5) 2_655 . . 3_665 ?
C6 C7 C8 C7 -178.80(17) . . . 3_665 ?
C8 C7 C8 C9 177.95(17) 2_655 . . . ?
C6 C7 C8 C9 -1.8(4) . . . . ?
C7 C8 C9 C10 87.9(3) 3_665 . . . ?
C7 C8 C9 C10 -89.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.265
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.110
