# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_10.H2O
_audit_block_doi                 10.5517/ccy38t3
_database_code_depnum_ccdc_archive 'CCDC 867095'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/ejoc.201200252 2012
_audit_update_record             
;
2015-08-23 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H24 O8 S4. (H2O)'
_chemical_formula_sum            'C40 H26 O9 S4'
_chemical_formula_weight         778.85

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

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   25.766(4)
_cell_length_b                   25.766(4)
_cell_length_c                   29.978(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     17236(6)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.86
_cell_measurement_theta_max      23.7

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             7236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    0.303
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9249
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32138
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.276
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9248
_reflns_number_gt                4548
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

DELU 0.005 C8 C13, C27 C28, C28 C29
ISOR 0.02 O9
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1836P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9248
_refine_ls_number_parameters     480
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0834
_refine_ls_wR_factor_ref         0.2932
_refine_ls_wR_factor_gt          0.2569
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.991
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.57844(5) 0.06211(5) 0.03523(4) 0.0670(3) Uani 1 1 d . . . . .
S2 S 0.74698(6) 0.14230(6) -0.09661(4) 0.0758(4) Uani 1 1 d . . . . .
S3 S 0.85839(5) 0.04045(5) -0.00321(4) 0.0725(3) Uani 1 1 d . . . . .
S4 S 0.68112(5) -0.05104(5) 0.12399(4) 0.0717(3) Uani 1 1 d . . . . .
O1 O 0.67463(14) 0.15189(13) -0.02541(10) 0.0722(8) Uani 1 1 d . . . . .
O2 O 0.72706(16) 0.15336(15) 0.03314(12) 0.0891(10) Uani 1 1 d . . . . .
O3 O 0.77761(13) 0.09538(14) -0.01841(9) 0.0707(8) Uani 1 1 d . . . . .
H3 H 0.7960 0.0961 0.0041 0.106 Uiso 1 1 calc R U . . .
O4 O 0.8994(2) 0.1161(3) -0.20499(16) 0.1532(19) Uani 1 1 d . . . . .
O5 O 0.80614(14) 0.02007(14) 0.08974(10) 0.0784(8) Uani 1 1 d . . . . .
O6 O 0.80632(15) 0.10269(15) 0.06759(11) 0.0846(9) Uani 1 1 d . . . . .
O7 O 0.67759(12) 0.04189(13) 0.06984(10) 0.0700(7) Uani 1 1 d . . . . .
H7 H 0.6757 0.0670 0.0542 0.105 Uiso 1 1 calc R U . . .
O8 O 0.4068(2) -0.1298(2) 0.12625(17) 0.1326(16) Uani 1 1 d . . . . .
C1 C 0.65484(17) 0.09310(18) -0.03612(12) 0.0581(9) Uani 1 1 d . . . . .
C2 C 0.68136(19) 0.0815(2) -0.07283(13) 0.0659(10) Uani 1 1 d . . . . .
C3 C 0.6584(2) 0.0237(2) -0.08725(15) 0.0775(12) Uani 1 1 d . . . . .
H3A H 0.6748 0.0154 -0.1120 0.093 Uiso 1 1 calc R U . . .
C4 C 0.6111(2) -0.0219(2) -0.06519(17) 0.0812(13) Uani 1 1 d . . . . .
H4 H 0.5955 -0.0610 -0.0755 0.097 Uiso 1 1 calc R U . . .
C5 C 0.58636(19) -0.0119(2) -0.02877(16) 0.0725(11) Uani 1 1 d . . . . .
H5 H 0.5549 -0.0439 -0.0140 0.087 Uiso 1 1 calc R U . . .
C6 C 0.60806(17) 0.04658(18) -0.01323(12) 0.0589(9) Uani 1 1 d . . . . .
C7 C 0.7170(2) 0.1795(2) 0.00462(17) 0.0751(12) Uani 1 1 d . . . . .
C8 C 0.7493(2) 0.2465(2) -0.00054(19) 0.0793(12) Uani 1 1 d . U . . .
C9 C 0.7419(3) 0.2717(3) -0.0362(2) 0.116(2) Uani 1 1 d . . . . .
H9 H 0.7158 0.2482 -0.0586 0.139 Uiso 1 1 calc R U . . .
C10 C 0.7743(4) 0.3356(4) -0.0404(3) 0.154(3) Uani 1 1 d . . . . .
H10 H 0.7677 0.3545 -0.0643 0.185 Uiso 1 1 calc R U . . .
C11 C 0.8136(4) 0.3666(3) -0.0093(4) 0.153(3) Uani 1 1 d . . . . .
H11 H 0.8368 0.4077 -0.0136 0.183 Uiso 1 1 calc R U . . .
C12 C 0.8233(3) 0.3442(3) 0.0279(3) 0.132(2) Uani 1 1 d . . . . .
H12 H 0.8497 0.3687 0.0499 0.159 Uiso 1 1 calc R U . . .
C13 C 0.7895(3) 0.2785(3) 0.0320(2) 0.1038(17) Uani 1 1 d . U . . .
H13 H 0.7956 0.2594 0.0561 0.125 Uiso 1 1 calc R U . . .
C14 C 0.80600(18) 0.09124(17) -0.05448(12) 0.0614(9) Uani 1 1 d . . . . .
C15 C 0.79488(18) 0.11183(19) -0.09489(12) 0.0644(10) Uani 1 1 d . . . . .
C16 C 0.82564(19) 0.1123(2) -0.13325(14) 0.0739(11) Uani 1 1 d . . . . .
H16 H 0.8185 0.1257 -0.1601 0.089 Uiso 1 1 calc R U . . .
C17 C 0.8664(2) 0.0931(2) -0.13121(15) 0.0787(12) Uani 1 1 d . . . . .
C18 C 0.87490(19) 0.0693(2) -0.09165(15) 0.0744(11) Uani 1 1 d . . . . .
H18 H 0.9012 0.0545 -0.0911 0.089 Uiso 1 1 calc R U . . .
C19 C 0.84409(19) 0.0680(2) -0.05349(13) 0.0684(11) Uani 1 1 d . . . . .
C20 C 0.9014(3) 0.0953(3) -0.17087(18) 0.1077(19) Uani 1 1 d . . . . .
H20 H 0.9264 0.0791 -0.1686 0.129 Uiso 1 1 calc R U . . .
C21 C 0.76456(19) -0.01511(17) 0.05647(13) 0.0612(10) Uani 1 1 d . . . . .
C22 C 0.78424(18) -0.01335(17) 0.01288(13) 0.0616(9) Uani 1 1 d . . . . .
C23 C 0.7435(2) -0.0536(2) -0.01738(15) 0.0728(11) Uani 1 1 d . . . . .
H23 H 0.7554 -0.0535 -0.0467 0.087 Uiso 1 1 calc R U . . .
C24 C 0.6851(2) -0.0941(2) -0.00462(16) 0.0798(13) Uani 1 1 d . . . . .
H24 H 0.6584 -0.1211 -0.0253 0.096 Uiso 1 1 calc R U . . .
C25 C 0.6666(2) -0.09445(18) 0.03802(15) 0.0682(10) Uani 1 1 d . . . . .
H25 H 0.6276 -0.1218 0.0465 0.082 Uiso 1 1 calc R U . . .
C26 C 0.70706(18) -0.05327(17) 0.06909(13) 0.0595(9) Uani 1 1 d . . . . .
C27 C 0.8228(2) 0.0774(2) 0.09234(14) 0.0736(11) Uani 1 1 d . U . . .
C28 C 0.86849(18) 0.1089(2) 0.12823(13) 0.0662(10) Uani 1 1 d . U . . .
C29 C 0.8889(2) 0.1707(3) 0.13359(17) 0.0932(15) Uani 1 1 d . U . . .
H29 H 0.8736 0.1893 0.1157 0.112 Uiso 1 1 calc R U . . .
C30 C 0.9329(3) 0.2042(3) 0.16654(19) 0.111(2) Uani 1 1 d . . . . .
H30 H 0.9470 0.2448 0.1711 0.133 Uiso 1 1 calc R U . . .
C31 C 0.9537(3) 0.1727(4) 0.1915(2) 0.117(2) Uani 1 1 d . . . . .
H31 H 0.9828 0.1935 0.2131 0.141 Uiso 1 1 calc R U . . .
C32 C 0.9341(4) 0.1142(4) 0.1863(3) 0.140(3) Uani 1 1 d . . . . .
H32 H 0.9500 0.0956 0.2037 0.168 Uiso 1 1 calc R U . . .
C33 C 0.8901(3) 0.0813(3) 0.15485(19) 0.114(2) Uani 1 1 d . . . . .
H33 H 0.8755 0.0404 0.1520 0.137 Uiso 1 1 calc R U . . .
C34 C 0.62318(17) 0.00144(16) 0.08281(13) 0.0571(9) Uani 1 1 d . . . . .
C35 C 0.61679(18) -0.04592(18) 0.10929(12) 0.0607(9) Uani 1 1 d . . . . .
C36 C 0.5608(2) -0.0880(2) 0.12542(15) 0.0726(11) Uani 1 1 d . . . . .
H36 H 0.5572 -0.1189 0.1436 0.087 Uiso 1 1 calc R U . . .
C37 C 0.51018(19) -0.0845(2) 0.11479(14) 0.0701(11) Uani 1 1 d . . . . .
C38 C 0.51609(18) -0.03827(19) 0.08705(13) 0.0675(10) Uani 1 1 d . . . . .
H38 H 0.4824 -0.0357 0.0796 0.081 Uiso 1 1 calc R U . . .
C39 C 0.57158(19) 0.00362(18) 0.07057(13) 0.0629(10) Uani 1 1 d . . . . .
C40 C 0.4537(3) -0.1284(3) 0.13299(18) 0.0965(15) Uani 1 1 d . . . . .
H40 H 0.4531 -0.1579 0.1512 0.116 Uiso 1 1 calc R U . . .
O9 O 0.95298(12) 0.02526(12) 0.07432(16) 0.1047(14) Uani 1 1 d . U . . .


_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
S1 C39 1.777(4) . ?
S1 C6 1.777(4) . ?
S2 C15 1.764(4) . ?
S2 C2 1.781(4) . ?
S3 C22 1.776(4) . ?
S3 C19 1.781(4) . ?
S4 C35 1.783(4) . ?
S4 C26 1.788(4) . ?
O1 C7 1.316(6) . ?
O1 C1 1.373(5) . ?
O2 C7 1.194(5) . ?
O3 C14 1.339(4) . ?
O3 H3 0.8200 . ?
O4 C20 1.169(7) . ?
O5 C27 1.319(5) . ?
O5 C21 1.412(5) . ?
O6 C27 1.196(5) . ?
O7 C34 1.320(5) . ?
O7 H7 0.8200 . ?
O8 C40 1.207(7) . ?
C1 C6 1.384(5) . ?
C1 C2 1.403(5) . ?
C2 C3 1.370(6) . ?
C3 C4 1.367(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.353(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(6) . ?
C5 H5 0.9300 . ?
C7 C8 1.503(7) . ?
C8 C9 1.312(8) . ?
C8 C13 1.362(8) . ?
C9 C10 1.430(10) . ?
C9 H9 0.9300 . ?
C10 C11 1.313(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.335(11) . ?
C11 H11 0.9300 . ?
C12 C13 1.472(9) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C19 1.383(6) . ?
C14 C15 1.408(5) . ?
C15 C16 1.393(6) . ?
C16 C17 1.368(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.401(7) . ?
C17 C20 1.476(7) . ?
C18 C19 1.383(6) . ?
C18 H18 0.9300 . ?
C20 H20 0.9300 . ?
C21 C26 1.360(6) . ?
C21 C22 1.394(6) . ?
C22 C23 1.383(6) . ?
C23 C24 1.389(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.362(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.405(6) . ?
C25 H25 0.9300 . ?
C27 C28 1.499(6) . ?
C28 C33 1.359(7) . ?
C28 C29 1.415(7) . ?
C29 C30 1.425(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.393(9) . ?
C30 H30 0.9300 . ?
C31 C32 1.338(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.390(9) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C35 1.395(5) . ?
C34 C39 1.407(6) . ?
C35 C36 1.387(6) . ?
C36 C37 1.389(6) . ?
C36 H36 0.9300 . ?
C37 C38 1.397(6) . ?
C37 C40 1.432(7) . ?
C38 C39 1.382(6) . ?
C38 H38 0.9300 . ?
C40 H40 0.9300 . ?

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
C39 S1 C6 99.69(18) . . ?
C15 S2 C2 99.5(2) . . ?
C22 S3 C19 100.64(19) . . ?
C35 S4 C26 98.69(18) . . ?
C7 O1 C1 120.4(3) . . ?
C14 O3 H3 109.5 . . ?
C27 O5 C21 118.6(3) . . ?
C34 O7 H7 109.5 . . ?
O1 C1 C6 121.4(3) . . ?
O1 C1 C2 117.7(4) . . ?
C6 C1 C2 120.7(4) . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 S2 122.3(3) . . ?
C1 C2 S2 118.5(3) . . ?
C4 C3 C2 119.8(4) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C5 C4 C3 121.9(4) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C4 C5 C6 120.1(4) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 118.3(4) . . ?
C1 C6 S1 119.8(3) . . ?
C5 C6 S1 122.0(3) . . ?
O2 C7 O1 122.7(5) . . ?
O2 C7 C8 124.8(5) . . ?
O1 C7 C8 112.6(4) . . ?
C9 C8 C13 122.6(5) . . ?
C9 C8 C7 121.2(5) . . ?
C13 C8 C7 116.0(5) . . ?
C8 C9 C10 119.7(7) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 117.8(8) . . ?
C11 C10 H10 121.1 . . ?
C9 C10 H10 121.1 . . ?
C10 C11 C12 125.8(8) . . ?
C10 C11 H11 117.1 . . ?
C12 C11 H11 117.1 . . ?
C11 C12 C13 115.8(7) . . ?
C11 C12 H12 122.1 . . ?
C13 C12 H12 122.1 . . ?
C8 C13 C12 118.0(6) . . ?
C8 C13 H13 121.0 . . ?
C12 C13 H13 121.0 . . ?
O3 C14 C19 123.5(4) . . ?
O3 C14 C15 116.3(4) . . ?
C19 C14 C15 120.3(4) . . ?
C16 C15 C14 119.5(4) . . ?
C16 C15 S2 119.5(3) . . ?
C14 C15 S2 120.8(3) . . ?
C17 C16 C15 119.7(4) . . ?
C17 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
C16 C17 C18 120.8(4) . . ?
C16 C17 C20 121.0(5) . . ?
C18 C17 C20 118.2(5) . . ?
C19 C18 C17 119.8(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C14 C19 C18 119.6(4) . . ?
C14 C19 S3 121.6(3) . . ?
C18 C19 S3 118.7(3) . . ?
O4 C20 C17 123.7(7) . . ?
O4 C20 H20 118.1 . . ?
C17 C20 H20 118.1 . . ?
C26 C21 C22 122.1(4) . . ?
C26 C21 O5 118.1(3) . . ?
C22 C21 O5 119.6(4) . . ?
C23 C22 C21 117.6(4) . . ?
C23 C22 S3 121.6(3) . . ?
C21 C22 S3 120.8(3) . . ?
C22 C23 C24 120.9(4) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C25 C24 C23 120.5(4) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C21 C26 C25 119.3(4) . . ?
C21 C26 S4 121.5(3) . . ?
C25 C26 S4 119.1(3) . . ?
O6 C27 O5 124.6(4) . . ?
O6 C27 C28 123.2(5) . . ?
O5 C27 C28 112.1(4) . . ?
C33 C28 C29 120.2(5) . . ?
C33 C28 C27 123.8(5) . . ?
C29 C28 C27 116.1(4) . . ?
C28 C29 C30 119.8(6) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C31 C30 C29 116.1(6) . . ?
C31 C30 H30 121.9 . . ?
C29 C30 H30 121.9 . . ?
C32 C31 C30 123.7(6) . . ?
C32 C31 H31 118.1 . . ?
C30 C31 H31 118.1 . . ?
C31 C32 C33 119.9(7) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C28 C33 C32 120.2(7) . . ?
C28 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
O7 C34 C35 118.2(3) . . ?
O7 C34 C39 122.9(3) . . ?
C35 C34 C39 118.9(4) . . ?
C36 C35 C34 120.3(4) . . ?
C36 C35 S4 119.8(3) . . ?
C34 C35 S4 119.9(3) . . ?
C35 C36 C37 120.8(4) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C36 C37 C38 119.1(4) . . ?
C36 C37 C40 118.5(5) . . ?
C38 C37 C40 122.4(5) . . ?
C39 C38 C37 120.5(4) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C34 120.3(4) . . ?
C38 C39 S1 120.1(3) . . ?
C34 C39 S1 119.6(3) . . ?
O8 C40 C37 124.5(6) . . ?
O8 C40 H40 117.8 . . ?
C37 C40 H40 117.8 . . ?

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
C7 O1 C1 C6 89.4(5) . . . . ?
C7 O1 C1 C2 -94.1(4) . . . . ?
O1 C1 C2 C3 -173.2(4) . . . . ?
C6 C1 C2 C3 3.3(6) . . . . ?
O1 C1 C2 S2 11.0(5) . . . . ?
C6 C1 C2 S2 -172.5(3) . . . . ?
C15 S2 C2 C3 -49.2(4) . . . . ?
C15 S2 C2 C1 126.5(3) . . . . ?
C1 C2 C3 C4 -1.6(6) . . . . ?
S2 C2 C3 C4 174.1(4) . . . . ?
C2 C3 C4 C5 -0.8(7) . . . . ?
C3 C4 C5 C6 1.5(7) . . . . ?
O1 C1 C6 C5 173.7(4) . . . . ?
C2 C1 C6 C5 -2.6(5) . . . . ?
O1 C1 C6 S1 -7.6(5) . . . . ?
C2 C1 C6 S1 176.0(3) . . . . ?
C4 C5 C6 C1 0.2(6) . . . . ?
C4 C5 C6 S1 -178.4(3) . . . . ?
C39 S1 C6 C1 -136.5(3) . . . . ?
C39 S1 C6 C5 42.1(4) . . . . ?
C1 O1 C7 O2 -24.0(6) . . . . ?
C1 O1 C7 C8 157.5(4) . . . . ?
O2 C7 C8 C9 170.1(6) . . . . ?
O1 C7 C8 C9 -11.5(7) . . . . ?
O2 C7 C8 C13 -4.9(7) . . . . ?
O1 C7 C8 C13 173.5(4) . . . . ?
C13 C8 C9 C10 -4.0(10) . . . . ?
C7 C8 C9 C10 -178.7(6) . . . . ?
C8 C9 C10 C11 4.5(13) . . . . ?
C9 C10 C11 C12 -5.3(16) . . . . ?
C10 C11 C12 C13 4.9(15) . . . . ?
C9 C8 C13 C12 3.7(9) . . . . ?
C7 C8 C13 C12 178.7(5) . . . . ?
C11 C12 C13 C8 -3.8(10) . . . . ?
O3 C14 C15 C16 176.1(4) . . . . ?
C19 C14 C15 C16 -4.3(6) . . . . ?
O3 C14 C15 S2 1.0(5) . . . . ?
C19 C14 C15 S2 -179.4(3) . . . . ?
C2 S2 C15 C16 129.3(4) . . . . ?
C2 S2 C15 C14 -55.7(4) . . . . ?
C14 C15 C16 C17 -0.2(6) . . . . ?
S2 C15 C16 C17 174.9(4) . . . . ?
C15 C16 C17 C18 4.0(7) . . . . ?
C15 C16 C17 C20 -177.6(5) . . . . ?
C16 C17 C18 C19 -3.3(7) . . . . ?
C20 C17 C18 C19 178.3(5) . . . . ?
O3 C14 C19 C18 -175.4(4) . . . . ?
C15 C14 C19 C18 5.1(6) . . . . ?
O3 C14 C19 S3 0.5(6) . . . . ?
C15 C14 C19 S3 -179.0(3) . . . . ?
C17 C18 C19 C14 -1.3(6) . . . . ?
C17 C18 C19 S3 -177.3(4) . . . . ?
C22 S3 C19 C14 55.7(4) . . . . ?
C22 S3 C19 C18 -128.4(4) . . . . ?
C16 C17 C20 O4 4.5(9) . . . . ?
C18 C17 C20 O4 -177.1(6) . . . . ?
C27 O5 C21 C26 -104.6(4) . . . . ?
C27 O5 C21 C22 80.4(5) . . . . ?
C26 C21 C22 C23 -2.2(6) . . . . ?
O5 C21 C22 C23 172.6(4) . . . . ?
C26 C21 C22 S3 175.9(3) . . . . ?
O5 C21 C22 S3 -9.4(5) . . . . ?
C19 S3 C22 C23 45.7(4) . . . . ?
C19 S3 C22 C21 -132.2(3) . . . . ?
C21 C22 C23 C24 0.2(6) . . . . ?
S3 C22 C23 C24 -177.9(3) . . . . ?
C22 C23 C24 C25 0.7(7) . . . . ?
C23 C24 C25 C26 0.3(7) . . . . ?
C22 C21 C26 C25 3.3(6) . . . . ?
O5 C21 C26 C25 -171.6(3) . . . . ?
C22 C21 C26 S4 -175.2(3) . . . . ?
O5 C21 C26 S4 10.0(5) . . . . ?
C24 C25 C26 C21 -2.3(6) . . . . ?
C24 C25 C26 S4 176.2(3) . . . . ?
C35 S4 C26 C21 127.8(3) . . . . ?
C35 S4 C26 C25 -50.7(3) . . . . ?
C21 O5 C27 O6 -2.0(7) . . . . ?
C21 O5 C27 C28 -178.1(3) . . . . ?
O6 C27 C28 C33 -176.0(5) . . . . ?
O5 C27 C28 C33 0.1(6) . . . . ?
O6 C27 C28 C29 4.1(6) . . . . ?
O5 C27 C28 C29 -179.8(4) . . . . ?
C33 C28 C29 C30 1.0(7) . . . . ?
C27 C28 C29 C30 -179.2(4) . . . . ?
C28 C29 C30 C31 0.6(8) . . . . ?
C29 C30 C31 C32 -0.7(10) . . . . ?
C30 C31 C32 C33 -0.8(12) . . . . ?
C29 C28 C33 C32 -2.5(9) . . . . ?
C27 C28 C33 C32 177.6(6) . . . . ?
C31 C32 C33 C28 2.5(11) . . . . ?
O7 C34 C35 C36 177.0(4) . . . . ?
C39 C34 C35 C36 -3.9(6) . . . . ?
O7 C34 C35 S4 -0.9(5) . . . . ?
C39 C34 C35 S4 178.2(3) . . . . ?
C26 S4 C35 C36 124.0(3) . . . . ?
C26 S4 C35 C34 -58.1(3) . . . . ?
C34 C35 C36 C37 1.4(6) . . . . ?
S4 C35 C36 C37 179.3(3) . . . . ?
C35 C36 C37 C38 0.8(6) . . . . ?
C35 C36 C37 C40 -178.9(4) . . . . ?
C36 C37 C38 C39 -0.3(6) . . . . ?
C40 C37 C38 C39 179.3(4) . . . . ?
C37 C38 C39 C34 -2.2(6) . . . . ?
C37 C38 C39 S1 179.9(3) . . . . ?
O7 C34 C39 C38 -176.7(4) . . . . ?
C35 C34 C39 C38 4.3(6) . . . . ?
O7 C34 C39 S1 1.2(5) . . . . ?
C35 C34 C39 S1 -177.8(3) . . . . ?
C6 S1 C39 C38 -119.9(3) . . . . ?
C6 S1 C39 C34 62.2(3) . . . . ?
C36 C37 C40 O8 179.7(6) . . . . ?
C38 C37 C40 O8 0.1(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3 S3 0.82 2.64 3.080(3) 114.9 .
O3 H3 O6 0.82 1.92 2.663(4) 150.7 .
O7 H7 S1 0.82 2.51 3.034(3) 122.7 .
O7 H7 O2 0.82 2.04 2.725(4) 140.9 .
C36 H36 O8 0.93 2.74 3.657(6) 170.1 14
C18 H18 O9 0.93 3.04 3.872(5) 150.4 11_665
C18 H18 O9 0.93 3.06 3.897(6) 151.1 12_545
C11 H11 O1 0.93 2.85 3.693(8) 151.2 2_655

_refine_diff_density_max         1.186
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.090

_shelxl_version_number           2014-3


# start Validation Reply Form

_vrf_PLAT430_10.H2O              
;
PROBLEM:Short Inter D...A Contact O9 .. O9 .. 2.84 Ang.
RESPONSE: This is due to the unresolved disorder of the water solvent molecules as the
crystal data sets were collected at room temperature.
;

#===END
####################################################################### 
# 
# 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_11
_audit_block_doi                 10.5517/ccy38v4
_database_code_depnum_ccdc_archive 'CCDC 867096'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/ejoc.201200252 2012
_audit_update_record             
;
2015-08-23 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H22 O7 S4'
_chemical_formula_sum            'C30 H22 O7 S4'
_chemical_formula_weight         622.69

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

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   37.589(3)
_cell_length_b                   37.589(3)
_cell_length_c                   10.6810(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13070(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9899
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      30.78

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_F_000             5742
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_absorpt_coefficient_mu    0.374
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9326
_exptl_absorpt_correction_T_max  0.9496
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35903
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.877
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9252
_reflns_number_gt                6610
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

ISOR 0.02 O6, O6', C21, C21' 
SIMU 0.02 0.05 2.0 C17', C18', C19', C21', O6' 
DFIX 1.40 0.02 C15 C16, C16 C17, C18 C19 
DFIX 1.40 0.02 C15' C16', C16' C17', C19' C20' 
DFIX 1.35 0.02 C22 O7, O7 C28, C15' O5' 
DFIX 1.47 0.01 C18' C21' 
DFIX 1.20 0.02 C21' O6' 
DFIX 1.80 0.02 C23' S3', C27' S4', S4' C6 
DFIX 2.40 0.03 C18' O6' 
FLAT C17' C18' C19' C21' O6'
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXL'
_computing_publication_material  'Bruker SHELXL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1229P)²+41.9277P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9252
_refine_ls_number_parameters     524
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2377
_refine_ls_wR_factor_gt          0.2212
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.77851(3) 0.99933(2) 0.67723(7) 0.0438(2) Uani 1 1 d . . . . .
O1 O 0.78875(6) 0.94118(6) 0.84180(17) 0.0377(4) Uani 1 1 d . . . . .
H1 H 0.7883 0.9226 0.8834 0.057 Uiso 1 1 calc R U . . .
O2 O 0.66075(10) 1.00124(10) 0.9711(3) 0.0666(7) Uani 1 1 d . . . . .
O3 O 0.81535(8) 0.94891(9) 0.5816(2) 0.0545(6) Uani 1 1 d . . . . .
H3 H 0.8196 0.9633 0.6437 0.082 Uiso 1 1 calc R U . . .
O4 O 0.64619(9) 0.87353(9) 0.2939(2) 0.0562(6) Uani 1 1 d . . . . .
C1 C 0.76099(9) 0.95040(8) 0.8874(2) 0.0347(5) Uani 1 1 d . . . . .
C2 C 0.75150(9) 0.97633(7) 0.8175(2) 0.0359(5) Uani 1 1 d . . . . .
C3 C 0.72234(9) 0.98548(8) 0.8618(3) 0.0403(6) Uani 1 1 d . . . . .
H3A H 0.7165 1.0030 0.8159 0.048 Uiso 1 1 calc R U . . .
C4 C 0.70154(10) 0.96886(10) 0.9742(3) 0.0463(7) Uani 1 1 d . . . . .
C5 C 0.71092(12) 0.94391(13) 1.0422(3) 0.0548(8) Uani 1 1 d . . . . .
H5 H 0.6973 0.9329 1.1173 0.066 Uiso 1 1 calc R U . . .
C6 C 0.74046(10) 0.93454(10) 1.0015(2) 0.0440(7) Uani 1 1 d D . . . .
C7 C 0.66888(14) 0.97691(15) 1.0180(3) 0.0642(10) Uani 1 1 d . . . . .
H7 H 0.6534 0.9621 1.0868 0.077 Uiso 1 1 calc R U . . .
C8 C 0.77826(10) 0.93786(10) 0.5353(2) 0.0428(6) Uani 1 1 d . . . . .
C9 C 0.76092(11) 0.90525(11) 0.4470(2) 0.0468(7) Uani 1 1 d . . . . .
C10 C 0.72310(11) 0.89320(11) 0.3973(2) 0.0448(7) Uani 1 1 d . . . . .
H10 H 0.7115 0.8713 0.3414 0.054 Uiso 1 1 calc R U . . .
C11 C 0.70154(11) 0.91350(10) 0.4298(2) 0.0427(7) Uani 1 1 d . . . . .
C12 C 0.71813(10) 0.94540(9) 0.5162(2) 0.0409(6) Uani 1 1 d . . . . .
H12 H 0.7038 0.9587 0.5378 0.049 Uiso 1 1 calc R U . . .
C13 C 0.75602(10) 0.95744(9) 0.5703(2) 0.0390(6) Uani 1 1 d . . . . .
C14 C 0.66167(12) 0.90022(11) 0.3726(3) 0.0489(8) Uani 1 1 d . . . . .
H14 H 0.6472 0.9130 0.3981 0.059 Uiso 1 1 calc R U . . .
S2 S 0.78550(7) 0.87826(7) 0.38935(18) 0.0440(4) Uani 0.707(3) 1 d . . P A 1
S3 S 0.75203(6) 0.78296(4) 0.81487(11) 0.0539(5) Uani 0.707(3) 1 d . . P A 1
S4 S 0.75561(5) 0.90783(5) 1.09718(12) 0.0394(3) Uani 0.707(3) 1 d . . P A 1
O5 O 0.73220(14) 0.81286(14) 0.5837(4) 0.0463(9) Uani 0.707(3) 1 d . . P A 1
H5A H 0.7276 0.8194 0.5150 0.069 Uiso 0.707(3) 1 calc R U P A 1
O6 O 0.9196(4) 0.8909(7) 0.7588(14) 0.288(9) Uani 0.707(3) 1 d . U P A 1
O7 O 0.79105(13) 0.86826(16) 0.9425(4) 0.0395(10) Uani 0.707(3) 1 d D . P A 1
C15 C 0.7732(2) 0.8323(2) 0.6035(5) 0.0382(10) Uani 0.707(3) 1 d D . P A 1
C16 C 0.8018(2) 0.8633(2) 0.5237(5) 0.0395(11) Uani 0.707(3) 1 d D . P A 1
C17 C 0.84328(18) 0.8802(2) 0.5461(5) 0.0565(13) Uani 0.707(3) 1 d D . P A 1
H17 H 0.8622 0.9003 0.4928 0.068 Uiso 0.707(3) 1 calc R U P A 1
C18 C 0.8569(2) 0.8674(3) 0.6473(7) 0.071(3) Uani 0.707(3) 1 d D . P A 1
C19 C 0.8288(2) 0.8381(2) 0.7298(5) 0.0568(14) Uani 0.707(3) 1 d D . P A 1
H19 H 0.8383 0.8301 0.7985 0.068 Uiso 0.707(3) 1 calc R U P A 1
C20 C 0.78703(19) 0.82085(16) 0.7109(4) 0.0421(10) Uani 0.707(3) 1 d . . P A 1
C21 C 0.9023(3) 0.8864(4) 0.6688(9) 0.129(4) Uani 0.707(3) 1 d . U P A 1
H21 H 0.9185 0.8958 0.5973 0.155 Uiso 0.707(3) 1 calc R U P A 1
C22 C 0.74934(19) 0.84505(14) 0.9504(4) 0.0349(11) Uani 0.707(3) 1 d D . P A 1
C23 C 0.72695(16) 0.80702(12) 0.8883(4) 0.0398(9) Uani 0.707(3) 1 d . . P A 1
C24 C 0.6847(3) 0.7860(2) 0.8928(10) 0.054(2) Uani 0.707(3) 1 d . . P A 1
H24 H 0.6703 0.7610 0.8509 0.064 Uiso 0.707(3) 1 calc R U P A 1
C25 C 0.66329(19) 0.80100(15) 0.9580(5) 0.0518(11) Uani 0.707(3) 1 d . . P A 1
H25 H 0.6347 0.7865 0.9590 0.062 Uiso 0.707(3) 1 calc R U P A 1
C26 C 0.68462(16) 0.83782(14) 1.0217(4) 0.0458(10) Uani 0.707(3) 1 d . . P A 1
H26 H 0.6706 0.8480 1.0673 0.055 Uiso 0.707(3) 1 calc R U P A 1
C27 C 0.72754(19) 0.85952(16) 1.0169(4) 0.0348(10) Uani 0.707(3) 1 d . . P A 1
C28 C 0.81618(14) 0.86392(11) 1.0415(3) 0.0594(10) Uani 0.707(3) 1 d D . P A 1
H28A H 0.8164 0.8385 1.0289 0.071 Uiso 0.707(3) 1 calc R U P A 1
H28B H 0.8039 0.8625 1.1225 0.071 Uiso 0.707(3) 1 calc R U P A 1
C29 C 0.85987(18) 0.89950(15) 1.0408(5) 0.0839(14) Uani 0.707(3) 1 d . . P A 1
H29A H 0.8597 0.9250 1.0517 0.101 Uiso 0.707(3) 1 calc R U P A 1
H29B H 0.8725 0.9006 0.9606 0.101 Uiso 0.707(3) 1 calc R U P A 1
C30 C 0.88578(19) 0.89503(18) 1.1476(6) 0.0942(16) Uani 0.707(3) 1 d . . P A 1
H30A H 0.8741 0.8954 1.2273 0.141 Uiso 0.707(3) 1 calc R U P A 1
H30B H 0.9135 0.9174 1.1433 0.141 Uiso 0.707(3) 1 calc R U P A 1
H30C H 0.8856 0.8695 1.1378 0.141 Uiso 0.707(3) 1 calc R U P A 1
S2' S 0.79623(15) 0.89296(15) 0.3728(4) 0.0359(8) Uani 0.293(3) 1 d . . P A 2
S3' S 0.78553(16) 0.79628(10) 0.7800(3) 0.0593(13) Uani 0.293(3) 1 d D . P A 2
S4' S 0.75188(15) 0.89511(11) 1.0846(4) 0.0394(3) Uani 0.293(3) 1 d D . P A 2
O5' O 0.7536(5) 0.8213(3) 0.5654(10) 0.049(2) Uani 0.293(3) 1 d D . P A 2
H5' H 0.7426 0.8340 0.5384 0.074 Uiso 0.293(3) 1 calc R U P A 2
O6' O 0.9472(8) 0.9231(11) 0.685(3) 0.297(18) Uani 0.293(3) 1 d D U P A 2
O7' O 0.8043(4) 0.8730(5) 0.9271(13) 0.0395(10) Uani 0.293(3) 1 d . . P A 2
C15' C 0.7941(5) 0.8472(4) 0.5786(12) 0.040(3) Uani 0.293(3) 1 d D . P A 2
C16' C 0.8179(4) 0.8803(4) 0.5011(13) 0.039(3) Uani 0.293(3) 1 d D . P A 2
C17' C 0.8610(4) 0.9044(6) 0.5193(15) 0.064(4) Uani 0.293(3) 1 d D U P A 2
H17' H 0.8763 0.9272 0.4686 0.076 Uiso 0.293(3) 1 calc R U P A 2
C18' C 0.8810(4) 0.8943(5) 0.6146(16) 0.081(4) Uani 0.293(3) 1 d D U P A 2
C19' C 0.8558(6) 0.8627(6) 0.697(2) 0.065(5) Uani 0.293(3) 1 d D U P A 2
H19' H 0.8681 0.8580 0.7662 0.078 Uiso 0.293(3) 1 calc R U P A 2
C20' C 0.8128(5) 0.8376(4) 0.6825(10) 0.044(3) Uani 0.293(3) 1 d D . P A 2
C21' C 0.9257(3) 0.9056(5) 0.6033(12) 0.067(4) Uani 0.293(3) 1 d D U P A 2
H21' H 0.9354 0.8987 0.5327 0.081 Uiso 0.293(3) 1 calc R U P A 2
C22' C 0.7637(3) 0.8441(3) 0.9252(9) 0.042(3) Uani 0.293(3) 1 d G . P A 2
C23' C 0.7501(3) 0.8086(2) 0.8559(8) 0.050(3) Uani 0.293(3) 1 d DG . P A 2
C24' C 0.7085(4) 0.7808(3) 0.8469(10) 0.067(4) Uani 0.293(3) 1 d G . P A 2
H24' H 0.6993 0.7569 0.8003 0.080 Uiso 0.293(3) 1 calc R U P A 2
C25' C 0.6805(4) 0.7885(3) 0.9074(12) 0.063(11) Uani 0.293(3) 1 d G . P A 2
H25' H 0.6525 0.7698 0.9013 0.076 Uiso 0.293(3) 1 calc R U P A 2
C26' C 0.6941(4) 0.8241(3) 0.9767(10) 0.068(4) Uani 0.293(3) 1 d G . P A 2
H26' H 0.6753 0.8293 1.0174 0.081 Uiso 0.293(3) 1 calc R U P A 2
C27' C 0.7358(3) 0.8519(3) 0.9857(8) 0.040(3) Uani 0.293(3) 1 d DG . P A 2
C28' C 0.81618(14) 0.86392(11) 1.0415(3) 0.0594(10) Uani 0.293(3) 1 d . . P A 2
H28C H 0.8149 0.8375 1.0405 0.071 Uiso 0.293(3) 1 calc R U P A 2
H28D H 0.8004 0.8652 1.1113 0.071 Uiso 0.293(3) 1 calc R U P A 2
C29' C 0.85987(18) 0.89950(15) 1.0408(5) 0.0839(14) Uani 0.293(3) 1 d . . P A 2
H29C H 0.8597 0.9250 1.0517 0.101 Uiso 0.293(3) 1 calc R U P A 2
H29D H 0.8725 0.9006 0.9606 0.101 Uiso 0.293(3) 1 calc R U P A 2
C30' C 0.88578(19) 0.89503(18) 1.1476(6) 0.0942(16) Uani 0.293(3) 1 d . . P A 2
H30D H 0.8706 0.8884 1.2247 0.141 Uiso 0.293(3) 1 calc R U P A 2
H30E H 0.9112 0.9204 1.1570 0.141 Uiso 0.293(3) 1 calc R U P A 2
H30F H 0.8914 0.8735 1.1267 0.141 Uiso 0.293(3) 1 calc R U 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
S1 C2 1.774(3) . ?
S1 C13 1.779(3) . ?
O1 C1 1.345(4) . ?
O2 C7 1.208(5) . ?
O3 C8 1.335(4) . ?
O4 C14 1.212(4) . ?
C1 C6 1.406(4) . ?
C1 C2 1.408(4) . ?
C2 C3 1.386(4) . ?
C3 C4 1.398(4) . ?
C4 C5 1.365(5) . ?
C4 C7 1.480(5) . ?
C5 C6 1.392(5) . ?
C6 S4 1.717(3) . ?
C6 S4' 1.951(5) . ?
C8 C13 1.413(4) . ?
C8 C9 1.420(5) . ?
C9 C10 1.366(5) . ?
C9 S2 1.789(4) . ?
C9 S2' 1.793(5) . ?
C10 C11 1.406(4) . ?
C11 C12 1.390(4) . ?
C11 C14 1.456(5) . ?
C12 C13 1.387(4) . ?
S2 C16 1.760(7) . ?
S3 C20 1.766(6) . ?
S3 C23 1.782(5) . ?
S4 C27 1.797(5) . ?
O5 C15 1.352(7) . ?
O6 C21 1.125(13) . ?
O7 C22 1.363(7) . ?
O7 C28 1.480(6) . ?
C15 C16 1.409(8) . ?
C15 C20 1.412(7) . ?
C16 C17 1.379(7) . ?
C17 C18 1.380(10) . ?
C18 C19 1.393(11) . ?
C18 C21 1.504(11) . ?
C19 C20 1.380(8) . ?
C22 C27 1.385(7) . ?
C22 C23 1.411(6) . ?
C23 C24 1.375(12) . ?
C24 C25 1.382(13) . ?
C25 C26 1.383(7) . ?
C26 C27 1.398(8) . ?
C28 C29 1.513(7) . ?
C29 C30 1.562(8) . ?
S2' C16' 1.777(14) . ?
S3' C20' 1.718(14) . ?
S3' C23' 1.805(10) . ?
S4' C27' 1.772(10) . ?
O5' C15' 1.344(14) . ?
O6' C21' 1.146(18) . ?
O7' C22' 1.358(16) . ?
C15' C16' 1.385(14) . ?
C15' C20' 1.453(16) . ?
C16' C17' 1.419(15) . ?
C17' C18' 1.43(2) . ?
C18' C19' 1.40(3) . ?
C18' C21' 1.520(9) . ?
C19' C20' 1.417(17) . ?
C22' C27' 1.383(7) . ?
C22' C23' 1.383(7) . ?
C23' C24' 1.383(7) . ?
C24' C25' 1.383(7) . ?
C25' C26' 1.383(7) . ?
C26' C27' 1.383(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
C2 S1 C13 102.00(12) . . ?
O1 C1 C6 122.5(3) . . ?
O1 C1 C2 119.0(2) . . ?
C6 C1 C2 118.5(3) . . ?
C3 C2 C1 119.8(3) . . ?
C3 C2 S1 119.9(2) . . ?
C1 C2 S1 120.3(2) . . ?
C2 C3 C4 121.2(3) . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 C7 119.9(3) . . ?
C3 C4 C7 121.0(3) . . ?
C4 C5 C6 121.4(3) . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 S4 120.1(2) . . ?
C1 C6 S4 119.4(3) . . ?
C5 C6 S4' 123.8(3) . . ?
C1 C6 S4' 115.7(3) . . ?
O2 C7 C4 125.0(4) . . ?
O3 C8 C13 122.5(3) . . ?
O3 C8 C9 118.1(3) . . ?
C13 C8 C9 119.3(3) . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 S2 115.2(2) . . ?
C8 C9 S2 125.0(3) . . ?
C10 C9 S2' 121.6(3) . . ?
C8 C9 S2' 115.9(3) . . ?
C9 C10 C11 120.7(3) . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 C14 121.0(3) . . ?
C10 C11 C14 119.0(3) . . ?
C13 C12 C11 120.2(3) . . ?
C12 C13 C8 119.9(3) . . ?
C12 C13 S1 120.8(2) . . ?
C8 C13 S1 119.2(2) . . ?
O4 C14 C11 124.1(3) . . ?
C16 S2 C9 105.2(2) . . ?
C20 S3 C23 103.72(19) . . ?
C6 S4 C27 96.2(2) . . ?
C22 O7 C28 118.6(4) . . ?
O5 C15 C16 122.9(5) . . ?
O5 C15 C20 117.2(6) . . ?
C16 C15 C20 119.9(6) . . ?
C17 C16 C15 119.7(6) . . ?
C17 C16 S2 119.2(6) . . ?
C15 C16 S2 120.9(4) . . ?
C16 C17 C18 120.3(7) . . ?
C17 C18 C19 120.3(6) . . ?
C17 C18 C21 119.0(9) . . ?
C19 C18 C21 120.7(8) . . ?
C20 C19 C18 120.9(6) . . ?
C19 C20 C15 118.7(6) . . ?
C19 C20 S3 120.1(4) . . ?
C15 C20 S3 121.1(5) . . ?
O6 C21 C18 129.5(13) . . ?
O7 C22 C27 119.8(5) . . ?
O7 C22 C23 122.1(5) . . ?
C27 C22 C23 118.0(5) . . ?
C24 C23 C22 119.9(6) . . ?
C24 C23 S3 118.3(6) . . ?
C22 C23 S3 121.5(4) . . ?
C23 C24 C25 121.6(7) . . ?
C24 C25 C26 119.5(6) . . ?
C25 C26 C27 119.2(5) . . ?
C22 C27 C26 121.8(5) . . ?
C22 C27 S4 118.5(5) . . ?
C26 C27 S4 119.7(4) . . ?
O7 C28 C29 111.7(3) . . ?
C28 C29 C30 111.1(4) . . ?
C16' S2' C9 103.1(5) . . ?
C20' S3' C23' 102.9(5) . . ?
C27' S4' C6 108.7(4) . . ?
O5' C15' C16' 125.3(10) . . ?
O5' C15' C20' 114.4(15) . . ?
C16' C15' C20' 120.3(14) . . ?
C15' C16' C17' 120.7(13) . . ?
C15' C16' S2' 121.6(9) . . ?
C17' C16' S2' 117.6(11) . . ?
C16' C17' C18' 120.8(15) . . ?
C19' C18' C17' 117.1(12) . . ?
C19' C18' C21' 118.1(14) . . ?
C17' C18' C21' 121.8(15) . . ?
C18' C19' C20' 123.8(13) . . ?
C19' C20' C15' 116.9(13) . . ?
C19' C20' S3' 120.1(12) . . ?
C15' C20' S3' 123.0(13) . . ?
O6' C21' C18' 118(2) . . ?
O7' C22' C27' 119.6(9) . . ?
O7' C22' C23' 120.3(9) . . ?
C27' C22' C23' 120.0 . . ?
C24' C23' C22' 120.0 . . ?
C24' C23' S3' 118.4(6) . . ?
C22' C23' S3' 121.6(6) . . ?
C25' C24' C23' 120.0 . . ?
C24' C25' C26' 120.0 . . ?
C27' C26' C25' 120.0 . . ?
C22' C27' C26' 120.0 . . ?
C22' C27' S4' 121.6(6) . . ?
C26' C27' S4' 118.3(6) . . ?

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
O1 C1 C2 C3 178.7(2) . . . . ?
C6 C1 C2 C3 -0.3(4) . . . . ?
O1 C1 C2 S1 -4.5(3) . . . . ?
C6 C1 C2 S1 176.6(2) . . . . ?
C13 S1 C2 C3 -107.2(2) . . . . ?
C13 S1 C2 C1 76.0(2) . . . . ?
C1 C2 C3 C4 -1.0(4) . . . . ?
S1 C2 C3 C4 -177.9(2) . . . . ?
C2 C3 C4 C5 1.4(4) . . . . ?
C2 C3 C4 C7 -176.8(3) . . . . ?
C3 C4 C5 C6 -0.4(5) . . . . ?
C7 C4 C5 C6 177.7(3) . . . . ?
C4 C5 C6 C1 -0.9(5) . . . . ?
C4 C5 C6 S4 172.7(3) . . . . ?
C4 C5 C6 S4' -173.9(3) . . . . ?
O1 C1 C6 C5 -177.7(3) . . . . ?
C2 C1 C6 C5 1.2(4) . . . . ?
O1 C1 C6 S4 8.6(4) . . . . ?
C2 C1 C6 S4 -172.4(2) . . . . ?
O1 C1 C6 S4' -4.2(4) . . . . ?
C2 C1 C6 S4' 174.8(2) . . . . ?
C5 C4 C7 O2 173.0(4) . . . . ?
C3 C4 C7 O2 -8.9(6) . . . . ?
O3 C8 C9 C10 -179.8(3) . . . . ?
C13 C8 C9 C10 -0.1(4) . . . . ?
O3 C8 C9 S2 -1.6(4) . . . . ?
C13 C8 C9 S2 178.1(2) . . . . ?
O3 C8 C9 S2' -18.1(4) . . . . ?
C13 C8 C9 S2' 161.6(3) . . . . ?
C8 C9 C10 C11 1.9(5) . . . . ?
S2 C9 C10 C11 -176.5(2) . . . . ?
S2' C9 C10 C11 -158.8(3) . . . . ?
C9 C10 C11 C12 -2.0(4) . . . . ?
C9 C10 C11 C14 178.7(3) . . . . ?
C10 C11 C12 C13 0.3(4) . . . . ?
C14 C11 C12 C13 179.6(3) . . . . ?
C11 C12 C13 C8 1.5(4) . . . . ?
C11 C12 C13 S1 177.9(2) . . . . ?
O3 C8 C13 C12 178.1(3) . . . . ?
C9 C8 C13 C12 -1.6(4) . . . . ?
O3 C8 C13 S1 1.6(4) . . . . ?
C9 C8 C13 S1 -178.1(2) . . . . ?
C2 S1 C13 C12 79.2(2) . . . . ?
C2 S1 C13 C8 -104.4(2) . . . . ?
C12 C11 C14 O4 177.6(3) . . . . ?
C10 C11 C14 O4 -3.1(5) . . . . ?
C10 C9 S2 C16 -130.8(3) . . . . ?
C8 C9 S2 C16 50.9(4) . . . . ?
S2' C9 S2 C16 112.6(8) . . . . ?
C5 C6 S4 C27 104.2(3) . . . . ?
C1 C6 S4 C27 -82.2(3) . . . . ?
S4' C6 S4 C27 -7.3(9) . . . . ?
O5 C15 C16 C17 -176.6(5) . . . . ?
C20 C15 C16 C17 4.6(7) . . . . ?
O5 C15 C16 S2 -1.1(7) . . . . ?
C20 C15 C16 S2 -179.8(4) . . . . ?
C9 S2 C16 C17 -113.5(4) . . . . ?
C9 S2 C16 C15 70.9(5) . . . . ?
C15 C16 C17 C18 -1.0(9) . . . . ?
S2 C16 C17 C18 -176.7(6) . . . . ?
C16 C17 C18 C19 -1.9(11) . . . . ?
C16 C17 C18 C21 179.8(7) . . . . ?
C17 C18 C19 C20 1.2(11) . . . . ?
C21 C18 C19 C20 179.5(7) . . . . ?
C18 C19 C20 C15 2.4(8) . . . . ?
C18 C19 C20 S3 178.6(5) . . . . ?
O5 C15 C20 C19 175.9(4) . . . . ?
C16 C15 C20 C19 -5.3(7) . . . . ?
O5 C15 C20 S3 -0.2(6) . . . . ?
C16 C15 C20 S3 178.6(4) . . . . ?
C23 S3 C20 C19 114.1(4) . . . . ?
C23 S3 C20 C15 -69.8(4) . . . . ?
C17 C18 C21 O6 151.9(19) . . . . ?
C19 C18 C21 O6 -26(2) . . . . ?
C28 O7 C22 C27 88.1(6) . . . . ?
C28 O7 C22 C23 -94.6(5) . . . . ?
O7 C22 C23 C24 -175.9(6) . . . . ?
C27 C22 C23 C24 1.4(7) . . . . ?
O7 C22 C23 S3 9.7(6) . . . . ?
C27 C22 C23 S3 -173.0(4) . . . . ?
C20 S3 C23 C24 130.3(5) . . . . ?
C20 S3 C23 C22 -55.2(4) . . . . ?
C22 C23 C24 C25 -0.5(9) . . . . ?
S3 C23 C24 C25 174.0(5) . . . . ?
C23 C24 C25 C26 -0.8(10) . . . . ?
C24 C25 C26 C27 1.2(8) . . . . ?
O7 C22 C27 C26 176.4(5) . . . . ?
C23 C22 C27 C26 -0.9(7) . . . . ?
O7 C22 C27 S4 -2.9(7) . . . . ?
C23 C22 C27 S4 179.7(3) . . . . ?
C25 C26 C27 C22 -0.3(7) . . . . ?
C25 C26 C27 S4 179.0(4) . . . . ?
C6 S4 C27 C22 110.6(4) . . . . ?
C6 S4 C27 C26 -68.7(4) . . . . ?
C22 O7 C28 C29 -163.4(5) . . . . ?
O7 C28 C29 C30 178.7(4) . . . . ?
C10 C9 S2' C16' -139.8(5) . . . . ?
C8 C9 S2' C16' 58.9(6) . . . . ?
S2 C9 S2' C16' -67.8(8) . . . . ?
O5' C15' C16' C17' -176.6(12) . . . . ?
C20' C15' C16' C17' 2.0(19) . . . . ?
O5' C15' C16' S2' 1.3(18) . . . . ?
C20' C15' C16' S2' 179.9(8) . . . . ?
C9 S2' C16' C15' 62.6(11) . . . . ?
C9 S2' C16' C17' -119.4(11) . . . . ?
C15' C16' C17' C18' 3(2) . . . . ?
S2' C16' C17' C18' -175.4(9) . . . . ?
C16' C17' C18' C19' -7.3(17) . . . . ?
C16' C17' C18' C21' 152.5(15) . . . . ?
C17' C18' C19' C20' 8(2) . . . . ?
C21' C18' C19' C20' -152.6(16) . . . . ?
C18' C19' C20' C15' -4(2) . . . . ?
C18' C19' C20' S3' 173.1(12) . . . . ?
O5' C15' C20' C19' 177.2(13) . . . . ?
C16' C15' C20' C19' -1.5(18) . . . . ?
O5' C15' C20' S3' 0.6(14) . . . . ?
C16' C15' C20' S3' -178.2(9) . . . . ?
C23' S3' C20' C19' 119.0(12) . . . . ?
C23' S3' C20' C15' -64.5(9) . . . . ?
C19' C18' C21' O6' -73(3) . . . . ?
C17' C18' C21' O6' 128(3) . . . . ?
O7' C22' C23' C24' -175.2(12) . . . . ?
C27' C22' C23' C24' 0.0 . . . . ?
O7' C22' C23' S3' 7.0(11) . . . . ?
C27' C22' C23' S3' -177.8(6) . . . . ?
C20' S3' C23' C24' 123.5(7) . . . . ?
C20' S3' C23' C22' -58.7(7) . . . . ?
C22' C23' C24' C25' 0.0 . . . . ?
S3' C23' C24' C25' 177.8(6) . . . . ?
C23' C24' C25' C26' 0.0 . . . . ?
C24' C25' C26' C27' 0.0 . . . . ?
O7' C22' C27' C26' 175.3(12) . . . . ?
C23' C22' C27' C26' 0.0 . . . . ?
O7' C22' C27' S4' -9.4(10) . . . . ?
C23' C22' C27' S4' 175.4(7) . . . . ?
C25' C26' C27' C22' 0.0 . . . . ?
C25' C26' C27' S4' -175.5(7) . . . . ?
C6 S4' C27' C22' 108.7(5) . . . . ?
C6 S4' C27' C26' -75.8(6) . . . . ?

_refine_diff_density_max         1.334
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.089

_shelxl_version_number           2013-2


# start Validation Reply Form

_vrf_PLAT220_11                  
;
PROBLEM: Hirshfeld Test Diff for    O5     --  C16     ..        8.0 su    
RESPONSE: This should be omitted because of some unresolved disorder 
;


####################################################################### 
# 
# 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_7.CHCl3
_database_code_depnum_ccdc_archive 'CCDC 1056803'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H28 O5 S4, 0.17 (CHCl3)'
_chemical_formula_sum            'C31.17 H28.17 Cl0.51 O5 S4'
_chemical_formula_weight         628.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-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                   36.329(5)
_cell_length_b                   36.329(5)
_cell_length_c                   11.8166(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13506(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9938
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      31.04

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5793
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9296
_exptl_absorpt_correction_T_max  0.9296
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'

_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_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31597
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.84
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5286
_reflns_number_gt                4692
_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. 

SADI C26 S3 C26 S3' C19 S3 C19 S3' C28 S4 C28' S4 
DIFX 2.90 0.02 Cl1 Cl2 
DIFX 1.73 0.01 C32 Cl1 C32 Cl2 
DFIX 0.82 0.01 O2 H2 O4 H4 O4' H4' 
;

_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)+(0.1209P)²+116.6168P] 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         5286
_refine_ls_number_parameters     430
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0753
_refine_ls_wR_factor_ref         0.2301
_refine_ls_wR_factor_gt          0.2209
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.253
_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
C1 C 0.51065(14) 0.08554(15) 0.4462(4) 0.0267(10) Uani 1 1 d . . .
C2 C 0.47855(15) 0.06174(16) 0.5238(4) 0.0288(10) Uani 1 1 d . A .
C3 C 0.45334(15) 0.01814(17) 0.5084(4) 0.0329(11) Uani 1 1 d . . .
H3 H 0.4317 0.0018 0.5619 0.040 Uiso 1 1 calc R . .
C4 C 0.45929(16) -0.00203(16) 0.4159(4) 0.0348(11) Uani 1 1 d . . .
H4A H 0.4419 -0.0319 0.4061 0.042 Uiso 1 1 calc R . .
C5 C 0.49081(16) 0.02182(17) 0.3383(4) 0.0324(11) Uani 1 1 d . . .
H5 H 0.4947 0.0083 0.2744 0.039 Uiso 1 1 calc R . .
C6 C 0.51684(14) 0.06534(16) 0.3527(4) 0.0281(10) Uani 1 1 d . . .
C7 C 0.52532(18) 0.15690(17) 0.4145(5) 0.0403(12) Uani 1 1 d . . .
H7A H 0.4976 0.1510 0.4461 0.048 Uiso 1 1 calc R . .
H7B H 0.5223 0.1530 0.3314 0.048 Uiso 1 1 calc R . .
C8 C 0.5593(2) 0.2018(2) 0.4424(6) 0.0589(17) Uani 1 1 d . . .
H8A H 0.5870 0.2065 0.4145 0.071 Uiso 1 1 calc R . .
H8B H 0.5529 0.2219 0.4019 0.071 Uiso 1 1 calc R . .
C9 C 0.5630(3) 0.2116(3) 0.5657(7) 0.078(2) Uani 1 1 d . . .
H9A H 0.5366 0.2098 0.5926 0.116 Uiso 1 1 calc R . .
H9B H 0.5868 0.2404 0.5786 0.116 Uiso 1 1 calc R . .
H9C H 0.5680 0.1911 0.6069 0.116 Uiso 1 1 calc R . .
C10 C 0.59902(14) 0.08706(15) 0.2903(4) 0.0270(10) Uani 1 1 d . . .
C11 C 0.62300(15) 0.10522(16) 0.3897(4) 0.0304(10) Uani 1 1 d . . .
C12 C 0.65883(15) 0.10105(16) 0.4109(4) 0.0318(11) Uani 1 1 d . . .
C13 C 0.67024(15) 0.07979(16) 0.3341(4) 0.0339(11) Uani 1 1 d . . .
H13 H 0.6947 0.0774 0.3483 0.041 Uiso 1 1 calc R . .
C14 C 0.64660(15) 0.06187(15) 0.2363(4) 0.0326(11) Uani 1 1 d . . .
C15 C 0.61079(15) 0.06564(15) 0.2153(4) 0.0289(10) Uani 1 1 d . . .
H15 H 0.5944 0.0534 0.1490 0.035 Uiso 1 1 calc R . .
C16 C 0.66005(18) 0.04037(17) 0.1577(5) 0.0427(13) Uani 1 1 d . . .
H16 H 0.6854 0.0402 0.1754 0.051 Uiso 1 1 calc R . .
C17 C 0.66333(14) 0.10045(16) 0.6456(4) 0.0326(11) Uani 1 1 d . . .
C18 C 0.64613(15) 0.11807(17) 0.7203(5) 0.0369(12) Uani 1 1 d . A .
C19 C 0.62468(16) 0.09574(19) 0.8177(4) 0.0385(12) Uani 1 1 d D . .
C20 C 0.62073(17) 0.0567(2) 0.8408(4) 0.0421(13) Uani 1 1 d . A .
H20 H 0.6064 0.0417 0.9073 0.050 Uiso 1 1 calc R . .
C21 C 0.63746(16) 0.03953(18) 0.7675(5) 0.0390(12) Uani 1 1 d . . .
H21 H 0.6344 0.0125 0.7834 0.047 Uiso 1 1 calc R A .
C22 C 0.65875(15) 0.06112(17) 0.6707(4) 0.0348(11) Uani 1 1 d . A .
H22 H 0.6703 0.0489 0.6212 0.042 Uiso 1 1 calc R . .
C23 C 0.6852(2) 0.1929(2) 0.7413(7) 0.0609(18) Uani 1 1 d . A .
H23A H 0.7114 0.1935 0.7150 0.073 Uiso 1 1 calc R . .
H23B H 0.6847 0.1920 0.8251 0.073 Uiso 1 1 calc R . .
C24 C 0.6846(3) 0.2317(2) 0.7005(8) 0.078(2) Uani 1 1 d . . .
H24A H 0.6576 0.2299 0.7242 0.094 Uiso 1 1 calc R . .
H24B H 0.7082 0.2572 0.7367 0.094 Uiso 1 1 calc R . .
C25 C 0.6888(3) 0.2367(3) 0.5778(10) 0.102(3) Uani 1 1 d . . .
H25A H 0.7165 0.2410 0.5545 0.153 Uiso 1 1 calc R . .
H25B H 0.6863 0.2614 0.5551 0.153 Uiso 1 1 calc R . .
H25C H 0.6662 0.2111 0.5413 0.153 Uiso 1 1 calc R . .
C26 C 0.5468(2) 0.0859(3) 0.8793(6) 0.0268(16) Uani 0.859(16) 1 d PGD A 1
C27 C 0.5319(2) 0.0944(3) 0.7800(7) 0.026(2) Uani 0.859(16) 1 d PG A 1
C28 C 0.4885(3) 0.0737(4) 0.7580(8) 0.028(2) Uani 0.859(16) 1 d PGD A 1
C29 C 0.4600(2) 0.0446(3) 0.8354(8) 0.0286(18) Uani 0.859(16) 1 d PG A 1
H29 H 0.4304 0.0305 0.8204 0.034 Uiso 0.859(16) 1 calc PR A 1
C30 C 0.4749(2) 0.0361(2) 0.9348(5) 0.0304(18) Uani 0.859(16) 1 d PG A 1
H30 H 0.4554 0.0162 0.9877 0.036 Uiso 0.859(16) 1 calc PR A 1
C31 C 0.5183(3) 0.0568(3) 0.9567(4) 0.0283(16) Uani 0.859(16) 1 d PG A 1
H31 H 0.5285 0.0510 1.0246 0.034 Uiso 0.859(16) 1 calc PR A 1
S3 S 0.60160(9) 0.11579(15) 0.9178(3) 0.0371(9) Uani 0.859(16) 1 d PD A 1
O4 O 0.5587(3) 0.1232(3) 0.7027(7) 0.0326(16) Uani 0.859(16) 1 d PD A 1
H4 H 0.5835 0.1360 0.7293 0.039 Uiso 0.859(16) 1 calc PRD A 1
C26' C 0.5611(12) 0.1043(15) 0.860(3) 0.027(10) Uani 0.141(16) 1 d PG A 2
C27' C 0.5412(15) 0.1055(18) 0.761(4) 0.026(11) Uani 0.141(16) 1 d PG A 2
C28' C 0.4973(16) 0.080(2) 0.750(5) 0.028(14) Uani 0.141(16) 1 d PGD A 2
C29' C 0.4734(12) 0.0538(18) 0.838(5) 0.029(12) Uani 0.141(16) 1 d PG A 2
H29' H 0.4435 0.0366 0.8310 0.034 Uiso 0.141(16) 1 calc PR A 2
C30' C 0.4934(15) 0.0527(15) 0.938(3) 0.030(11) Uani 0.141(16) 1 d PG A 2
H30' H 0.4770 0.0346 0.9981 0.036 Uiso 0.141(16) 1 calc PR A 2
C31' C 0.5372(15) 0.0779(16) 0.949(2) 0.028(10) Uani 0.141(16) 1 d PG A 2
H31' H 0.5508 0.0772 1.0164 0.034 Uiso 0.141(16) 1 calc PR A 2
O4' O 0.5672(17) 0.1370(16) 0.675(5) 0.033(10) Uani 0.141(16) 1 d PD A 2
H4' H 0.5634 0.1249 0.6121 0.039 Uiso 0.141(16) 1 calc PRD A 2
S3' S 0.6113(5) 0.1342(8) 0.8807(19) 0.037(5) Uani 0.141(16) 1 d PD A 2
O1 O 0.53807(10) 0.12812(11) 0.4640(3) 0.0310(7) Uani 1 1 d . . .
O2 O 0.61390(11) 0.12767(12) 0.4626(3) 0.0351(8) Uani 1 1 d D . .
H2 H 0.5918(11) 0.128(2) 0.449(5) 0.042 Uiso 1 1 d D . .
O3 O 0.64800(12) 0.15575(12) 0.6960(4) 0.0476(10) Uani 1 1 d . . .
O5 O 0.64256(17) 0.02333(15) 0.0749(5) 0.0666(13) Uani 1 1 d . . .
S1 S 0.55700(4) 0.09636(4) 0.25107(10) 0.0333(4) Uani 1 1 d . . .
S2 S 0.69370(4) 0.12895(5) 0.52573(11) 0.0449(4) Uani 1 1 d . . .
S4 S 0.46828(4) 0.08797(4) 0.63748(10) 0.0343(4) Uani 1 1 d D . .
Cl2 Cl 0.6667 0.3333 0.5196(11) 0.080(4) Uani 0.25 3 d SPD . .
C32 C 0.6667 0.3333 0.6631(13) 0.065(6) Uani 0.50 3 d SPD . .
Cl1 Cl 0.6369(9) 0.2986(8) 0.7646(17) 0.098(9) Uani 0.08 1 d PD . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.374(6) . ?
C1 C2 1.393(7) . ?
C1 C6 1.405(6) . ?
C2 C3 1.389(7) . ?
C2 S4 1.791(5) . ?
C3 C4 1.392(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.389(7) . ?
C5 H5 0.9500 . ?
C6 S1 1.788(5) . ?
C7 O1 1.461(6) . ?
C7 C8 1.511(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.489(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C15 1.381(7) . ?
C10 C11 1.414(6) . ?
C10 S1 1.782(4) . ?
C11 O2 1.336(6) . ?
C11 C12 1.406(7) . ?
C12 C13 1.383(8) . ?
C12 S2 1.786(5) . ?
C13 C14 1.392(7) . ?
C13 H13 0.9500 . ?
C14 C15 1.396(7) . ?
C14 C16 1.447(8) . ?
C15 H15 0.9500 . ?
C16 O5 1.163(8) . ?
C16 H16 0.9500 . ?
C17 C22 1.386(8) . ?
C17 C18 1.407(8) . ?
C17 S2 1.775(5) . ?
C18 O3 1.367(7) . ?
C18 C19 1.400(8) . ?
C19 C20 1.379(9) . ?
C19 S3 1.801(5) . ?
C19 S3' 1.851(12) . ?
C20 C21 1.374(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(8) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 O3 1.453(7) . ?
C23 C24 1.503(11) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.460(14) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.3900 . ?
C26 C31 1.3900 . ?
C26 S3 1.786(6) . ?
C27 O4 1.363(7) . ?
C27 C28 1.3900 . ?
C28 C29 1.3900 . ?
C28 S4 1.794(4) . ?
C29 C30 1.3900 . ?
C29 H29 0.9500 . ?
C30 C31 1.3900 . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
O4 H4 0.8400 . ?
C26' C27' 1.3900 . ?
C26' C31' 1.3900 . ?
C26' S3' 1.61(3) . ?
C27' C28' 1.3900 . ?
C27' O4' 1.46(4) . ?
C28' C29' 1.3900 . ?
C28' S4 1.805(16) . ?
C29' C30' 1.3900 . ?
C29' H29' 0.9500 . ?
C30' C31' 1.3900 . ?
C30' H30' 0.9500 . ?
C31' H31' 0.9500 . ?
O4' H4' 0.8400 . ?
O2 H2 0.818(12) . ?
Cl2 C32 1.695(10) . ?
C32 Cl1 1.684(10) 3_665 ?
C32 Cl1 1.684(10) . ?
C32 Cl1 1.684(10) 2_655 ?
Cl1 Cl1 2.01(4) 17_556 ?
Cl1 Cl1 2.01(4) 18_546 ?
Cl1 Cl1 2.05(4) 3_665 ?
Cl1 Cl1 2.05(4) 2_655 ?

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
O1 C1 C2 120.6(4) . . ?
O1 C1 C6 119.5(4) . . ?
C2 C1 C6 119.8(4) . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 S4 120.7(4) . . ?
C1 C2 S4 119.8(4) . . ?
C2 C3 C4 121.0(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C4 C5 C6 120.8(4) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.7(4) . . ?
C5 C6 S1 120.8(4) . . ?
C1 C6 S1 119.5(4) . . ?
O1 C7 C8 107.8(4) . . ?
O1 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
O1 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.5 . . ?
C9 C8 C7 113.5(6) . . ?
C9 C8 H8A 108.9 . . ?
C7 C8 H8A 108.9 . . ?
C9 C8 H8B 108.9 . . ?
C7 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C15 C10 C11 120.2(4) . . ?
C15 C10 S1 118.4(3) . . ?
C11 C10 S1 120.9(4) . . ?
O2 C11 C12 118.4(4) . . ?
O2 C11 C10 122.5(4) . . ?
C12 C11 C10 119.1(4) . . ?
C13 C12 C11 119.6(4) . . ?
C13 C12 S2 119.4(4) . . ?
C11 C12 S2 120.4(4) . . ?
C12 C13 C14 121.3(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 119.4 . . ?
C13 C14 C15 119.3(5) . . ?
C13 C14 C16 119.3(5) . . ?
C15 C14 C16 121.4(5) . . ?
C10 C15 C14 120.5(4) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
O5 C16 C14 125.9(6) . . ?
O5 C16 H16 117.1 . . ?
C14 C16 H16 117.1 . . ?
C22 C17 C18 118.9(5) . . ?
C22 C17 S2 119.5(4) . . ?
C18 C17 S2 121.5(4) . . ?
O3 C18 C19 119.2(5) . . ?
O3 C18 C17 120.9(5) . . ?
C19 C18 C17 119.9(5) . . ?
C20 C19 C18 120.0(5) . . ?
C20 C19 S3 117.1(4) . . ?
C18 C19 S3 122.9(5) . . ?
C20 C19 S3' 140.0(10) . . ?
C18 C19 S3' 100.0(10) . . ?
S3 C19 S3' 22.9(8) . . ?
C21 C20 C19 120.0(5) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.8(5) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C17 120.5(5) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
O3 C23 C24 108.0(5) . . ?
O3 C23 H23A 110.1 . . ?
C24 C23 H23A 110.1 . . ?
O3 C23 H23B 110.1 . . ?
C24 C23 H23B 110.1 . . ?
H23A C23 H23B 108.4 . . ?
C25 C24 C23 112.7(8) . . ?
C25 C24 H24A 109.1 . . ?
C23 C24 H24A 109.1 . . ?
C25 C24 H24B 109.1 . . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C31 120.0 . . ?
C27 C26 S3 121.3(4) . . ?
C31 C26 S3 118.4(4) . . ?
O4 C27 C26 121.8(6) . . ?
O4 C27 C28 118.2(6) . . ?
C26 C27 C28 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 S4 119.0(5) . . ?
C27 C28 S4 120.7(5) . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 120.0 . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C26 120.0 . . ?
C30 C31 H31 120.0 . . ?
C26 C31 H31 120.0 . . ?
C26 S3 C19 100.9(3) . . ?
C27 O4 H4 109.5 . . ?
C27' C26' C31' 120.0 . . ?
C27' C26' S3' 123(2) . . ?
C31' C26' S3' 117(2) . . ?
C28' C27' C26' 120.0 . . ?
C28' C27' O4' 122(3) . . ?
C26' C27' O4' 118(3) . . ?
C27' C28' C29' 120.0 . . ?
C27' C28' S4 122(3) . . ?
C29' C28' S4 117(3) . . ?
C30' C29' C28' 120.0 . . ?
C30' C29' H29' 120.0 . . ?
C28' C29' H29' 120.0 . . ?
C31' C30' C29' 120.0 . . ?
C31' C30' H30' 120.0 . . ?
C29' C30' H30' 120.0 . . ?
C30' C31' C26' 120.0 . . ?
C30' C31' H31' 120.0 . . ?
C26' C31' H31' 120.0 . . ?
C27' O4' H4' 109.5 . . ?
C26' S3' C19 93.9(16) . . ?
C1 O1 C7 115.7(3) . . ?
C11 O2 H2 115(4) . . ?
C18 O3 C23 114.2(4) . . ?
C10 S1 C6 102.2(2) . . ?
C17 S2 C12 102.5(2) . . ?
C2 S4 C28 102.6(5) . . ?
C2 S4 C28' 100(3) . . ?
C28 S4 C28' 9.6(19) . . ?
Cl1 C32 Cl1 74.8(14) 3_665 . ?
Cl1 C32 Cl1 74.8(14) 3_665 2_655 ?
Cl1 C32 Cl1 74.8(14) . 2_655 ?
Cl1 C32 Cl2 135.5(9) 3_665 . ?
Cl1 C32 Cl2 135.5(9) . . ?
Cl1 C32 Cl2 135.5(9) 2_655 . ?
C32 Cl1 Cl1 111.7(9) . 17_556 ?
C32 Cl1 Cl1 111.7(9) . 18_546 ?
Cl1 Cl1 Cl1 61.3(9) 17_556 18_546 ?
C32 Cl1 Cl1 52.6(7) . 3_665 ?
Cl1 Cl1 Cl1 59.4(5) 17_556 3_665 ?
Cl1 Cl1 Cl1 89.999(5) 18_546 3_665 ?
C32 Cl1 Cl1 52.6(7) . 2_655 ?
Cl1 Cl1 Cl1 90.002(7) 17_556 2_655 ?
Cl1 Cl1 Cl1 59.4(5) 18_546 2_655 ?
Cl1 Cl1 Cl1 60.003(12) 3_665 2_655 ?

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
O1 C1 C2 C3 -175.1(4) . . . . ?
C6 C1 C2 C3 0.8(6) . . . . ?
O1 C1 C2 S4 8.4(6) . . . . ?
C6 C1 C2 S4 -175.7(3) . . . . ?
C1 C2 C3 C4 -0.9(7) . . . . ?
S4 C2 C3 C4 175.6(3) . . . . ?
C2 C3 C4 C5 0.0(7) . . . . ?
C3 C4 C5 C6 1.0(7) . . . . ?
C4 C5 C6 C1 -1.1(7) . . . . ?
C4 C5 C6 S1 -178.8(3) . . . . ?
O1 C1 C6 C5 176.1(4) . . . . ?
C2 C1 C6 C5 0.2(6) . . . . ?
O1 C1 C6 S1 -6.1(5) . . . . ?
C2 C1 C6 S1 178.0(3) . . . . ?
O1 C7 C8 C9 -65.3(7) . . . . ?
C15 C10 C11 O2 177.3(4) . . . . ?
S1 C10 C11 O2 4.5(6) . . . . ?
C15 C10 C11 C12 -0.1(7) . . . . ?
S1 C10 C11 C12 -172.9(4) . . . . ?
O2 C11 C12 C13 -176.8(4) . . . . ?
C10 C11 C12 C13 0.7(7) . . . . ?
O2 C11 C12 S2 -5.4(6) . . . . ?
C10 C11 C12 S2 172.2(4) . . . . ?
C11 C12 C13 C14 -0.8(7) . . . . ?
S2 C12 C13 C14 -172.4(4) . . . . ?
C12 C13 C14 C15 0.3(7) . . . . ?
C12 C13 C14 C16 179.3(5) . . . . ?
C11 C10 C15 C14 -0.4(7) . . . . ?
S1 C10 C15 C14 172.6(4) . . . . ?
C13 C14 C15 C10 0.3(7) . . . . ?
C16 C14 C15 C10 -178.6(5) . . . . ?
C13 C14 C16 O5 178.1(6) . . . . ?
C15 C14 C16 O5 -3.0(9) . . . . ?
C22 C17 C18 O3 -176.7(4) . . . . ?
S2 C17 C18 O3 7.7(6) . . . . ?
C22 C17 C18 C19 -0.3(7) . . . . ?
S2 C17 C18 C19 -175.9(3) . . . . ?
O3 C18 C19 C20 177.0(4) . . . . ?
C17 C18 C19 C20 0.5(7) . . . . ?
O3 C18 C19 S3 -3.4(6) . . . . ?
C17 C18 C19 S3 -179.9(3) . . . . ?
O3 C18 C19 S3' -4.9(6) . . . . ?
C17 C18 C19 S3' 178.7(5) . . . . ?
C18 C19 C20 C21 -0.7(7) . . . . ?
S3 C19 C20 C21 179.7(4) . . . . ?
S3' C19 C20 C21 -177.9(6) . . . . ?
C19 C20 C21 C22 0.7(8) . . . . ?
C20 C21 C22 C17 -0.5(7) . . . . ?
C18 C17 C22 C21 0.3(7) . . . . ?
S2 C17 C22 C21 176.0(4) . . . . ?
O3 C23 C24 C25 -64.3(10) . . . . ?
C31 C26 C27 O4 179.0(10) . . . . ?
S3 C26 C27 O4 5.8(10) . . . . ?
C31 C26 C27 C28 0.0 . . . . ?
S3 C26 C27 C28 -173.1(5) . . . . ?
O4 C27 C28 C29 -179.0(10) . . . . ?
C26 C27 C28 C29 0.0 . . . . ?
O4 C27 C28 S4 -5.2(7) . . . . ?
C26 C27 C28 S4 173.8(10) . . . . ?
C27 C28 C29 C30 0.0 . . . . ?
S4 C28 C29 C30 -173.9(10) . . . . ?
C28 C29 C30 C31 0.0 . . . . ?
C29 C30 C31 C26 0.0 . . . . ?
C27 C26 C31 C30 0.0 . . . . ?
S3 C26 C31 C30 173.3(5) . . . . ?
C27 C26 S3 C19 -72.5(5) . . . . ?
C31 C26 S3 C19 114.2(5) . . . . ?
C20 C19 S3 C26 -78.6(4) . . . . ?
C18 C19 S3 C26 101.8(4) . . . . ?
S3' C19 S3 C26 105.4(9) . . . . ?
C31' C26' C27' C28' 0.0 . . . . ?
S3' C26' C27' C28' -177(3) . . . . ?
C31' C26' C27' O4' 174(5) . . . . ?
S3' C26' C27' O4' -3(5) . . . . ?
C26' C27' C28' C29' 0.0 . . . . ?
O4' C27' C28' C29' -174(6) . . . . ?
C26' C27' C28' S4 167(6) . . . . ?
O4' C27' C28' S4 -7(4) . . . . ?
C27' C28' C29' C30' 0.0 . . . . ?
S4 C28' C29' C30' -168(5) . . . . ?
C28' C29' C30' C31' 0.0 . . . . ?
C29' C30' C31' C26' 0.0 . . . . ?
C27' C26' C31' C30' 0.0 . . . . ?
S3' C26' C31' C30' 177(3) . . . . ?
C27' C26' S3' C19 -89(3) . . . . ?
C31' C26' S3' C19 94(3) . . . . ?
C20 C19 S3' C26' -70.3(15) . . . . ?
C18 C19 S3' C26' 112.1(13) . . . . ?
S3 C19 S3' C26' -64.7(14) . . . . ?
C2 C1 O1 C7 -91.5(5) . . . . ?
C6 C1 O1 C7 92.7(5) . . . . ?
C8 C7 O1 C1 -179.7(5) . . . . ?
C19 C18 O3 C23 91.8(6) . . . . ?
C17 C18 O3 C23 -91.7(6) . . . . ?
C24 C23 O3 C18 175.7(6) . . . . ?
C15 C10 S1 C6 114.7(4) . . . . ?
C11 C10 S1 C6 -72.3(4) . . . . ?
C5 C6 S1 C10 -80.9(4) . . . . ?
C1 C6 S1 C10 101.3(4) . . . . ?
C22 C17 S2 C12 75.4(4) . . . . ?
C18 C17 S2 C12 -109.0(4) . . . . ?
C13 C12 S2 C17 -115.3(4) . . . . ?
C11 C12 S2 C17 73.2(4) . . . . ?
C3 C2 S4 C28 75.9(5) . . . . ?
C1 C2 S4 C28 -107.7(4) . . . . ?
C3 C2 S4 C28' 85.4(18) . . . . ?
C1 C2 S4 C28' -98.1(18) . . . . ?
C29 C28 S4 C2 -107.5(6) . . . . ?
C27 C28 S4 C2 78.6(6) . . . . ?
C29 C28 S4 C28' 176(20) . . . . ?
C27 C28 S4 C28' 2(19) . . . . ?
C27' C28' S4 C2 80(3) . . . . ?
C29' C28' S4 C2 -113(3) . . . . ?
C27' C28' S4 C28 -175(22) . . . . ?
C29' C28' S4 C28 -7(16) . . . . ?
Cl1 C32 Cl1 Cl1 -5.8(8) 3_665 . . 17_556 ?
Cl1 C32 Cl1 Cl1 72.3(5) 2_655 . . 17_556 ?
Cl2 C32 Cl1 Cl1 -146.7(5) . . . 17_556 ?
Cl1 C32 Cl1 Cl1 -72.3(5) 3_665 . . 18_546 ?
Cl1 C32 Cl1 Cl1 5.8(8) 2_655 . . 18_546 ?
Cl2 C32 Cl1 Cl1 146.7(5) . . . 18_546 ?
Cl1 C32 Cl1 Cl1 78.0(9) 2_655 . . 3_665 ?
Cl2 C32 Cl1 Cl1 -141.0(4) . . . 3_665 ?
Cl1 C32 Cl1 Cl1 -78.0(9) 3_665 . . 2_655 ?
Cl2 C32 Cl1 Cl1 141.0(4) . . . 2_655 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.122

# start Validation Reply Form

_vrf_PLAT230_7.CHCl3             
;
PROBLEM: Hirshfeld Test Diff for    O5     --  C16     ..        8.0 su    
RESPONSE: This should be omitted because of some unresolved disorder 
;

#===END
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 1056804'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H28 O6 S4'
_chemical_formula_sum            'C32 H28 O6 S4'
_chemical_formula_weight         636.78

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   'R-3   '
_symmetry_space_group_name_Hall  '-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                   36.0289(13)
_cell_length_b                   36.0289(13)
_cell_length_c                   12.2533(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13774.8(16)
_cell_formula_units_Z            18
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1825
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      23.66

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5976
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'TRIUMPH curved crystal monochromator'
_diffrn_measurement_device_type  'PHOTON100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13270
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_sigmaI/netI    0.1158
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.36
_reflns_number_total             5439
_reflns_number_gt                3077
_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. 

dfix .82 o1 h1a o4 h4a
sadi .02 o3 c14 o3 c14'
dfix 1.53 c14 c15 c15 c16 c14' c15' c15' c16'
sadi c9 c14 c9 c14'
sadi o3 c15 o3 c15'
sadi c14 c16 c14' c16'
simu .02 c14 > c16'
;

_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)+(0.0321P)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         5439
_refine_ls_number_parameters     413
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.0972
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.007
_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
C1 C 0.93166(9) 0.17903(9) 0.4630(3) 0.0236(8) Uani 1 1 d . . .
C2 C 0.95788(9) 0.18592(9) 0.5534(3) 0.0257(8) Uani 1 1 d . . .
C3 C 0.99346(9) 0.22744(10) 0.5725(3) 0.0276(9) Uani 1 1 d . . .
C4 C 1.00169(9) 0.26013(10) 0.5007(3) 0.0307(9) Uani 1 1 d . . .
H4 H 1.0252 0.2880 0.5144 0.037 Uiso 1 1 calc R . .
C5 C 0.97643(9) 0.25328(9) 0.4090(3) 0.0271(9) Uani 1 1 d . . .
C6 C 0.94128(9) 0.21249(9) 0.3909(3) 0.0281(8) Uani 1 1 d . . .
H6 H 0.9237 0.2075 0.3286 0.034 Uiso 1 1 calc R . .
C7 C 0.98617(10) 0.28770(10) 0.3302(3) 0.0378(10) Uani 1 1 d . . .
H7 H 0.9692 0.2806 0.2660 0.045 Uiso 1 1 calc R . .
C8 C 1.00253(9) 0.22664(10) 0.7994(3) 0.0283(9) Uani 1 1 d . . .
C9 C 0.98863(9) 0.18877(10) 0.8586(3) 0.0271(8) Uani 1 1 d D A .
C10 C 0.96892(9) 0.18388(10) 0.9588(3) 0.0290(9) Uani 1 1 d . . .
C11 C 0.96300(9) 0.21671(10) 0.9988(3) 0.0343(9) Uani 1 1 d . . .
H11 H 0.9503 0.2137 1.0686 0.041 Uiso 1 1 calc R . .
C12 C 0.97520(10) 0.25348(10) 0.9390(3) 0.0374(10) Uani 1 1 d . . .
H12 H 0.9699 0.2751 0.9660 0.045 Uiso 1 1 calc R . .
C13 C 0.99514(9) 0.25852(10) 0.8396(3) 0.0329(9) Uani 1 1 d . . .
H13 H 1.0039 0.2839 0.7984 0.039 Uiso 1 1 calc R . .
C17 C 0.89341(9) 0.11673(9) 1.0193(3) 0.0288(8) Uani 1 1 d . . .
C18 C 0.87205(10) 0.09508(10) 0.9233(3) 0.0276(8) Uani 1 1 d . . .
C19 C 0.82748(9) 0.07873(9) 0.9132(3) 0.0248(8) Uani 1 1 d . . .
C20 C 0.80564(10) 0.08489(9) 0.9968(3) 0.0261(8) Uani 1 1 d . . .
H20 H 0.7757 0.0742 0.9894 0.031 Uiso 1 1 calc R . .
C21 C 0.82641(10) 0.10660(9) 1.0925(3) 0.0265(8) Uani 1 1 d . . .
C22 C 0.87039(10) 0.12192(9) 1.1025(3) 0.0295(9) Uani 1 1 d . . .
H22 H 0.8848 0.1362 1.1676 0.035 Uiso 1 1 calc R . .
C23 C 0.80298(11) 0.11301(9) 1.1799(3) 0.0322(9) Uani 1 1 d . . .
H23 H 0.8180 0.1254 1.2457 0.039 Uiso 1 1 calc R . .
C24 C 0.80974(9) 0.08224(9) 0.6915(3) 0.0249(8) Uani 1 1 d . . .
C25 C 0.84235(9) 0.09031(9) 0.6171(3) 0.0239(8) Uani 1 1 d . . .
C26 C 0.84981(9) 0.11717(9) 0.5281(3) 0.0249(8) Uani 1 1 d . . .
C27 C 0.82385(10) 0.13518(9) 0.5139(3) 0.0298(9) Uani 1 1 d . . .
H27 H 0.8285 0.1534 0.4531 0.036 Uiso 1 1 calc R . .
C28 C 0.79123(10) 0.12707(10) 0.5869(3) 0.0343(10) Uani 1 1 d . . .
H28 H 0.7738 0.1397 0.5764 0.041 Uiso 1 1 calc R . .
C29 C 0.78431(9) 0.10058(9) 0.6747(3) 0.0294(9) Uani 1 1 d . . .
H29 H 0.7618 0.0948 0.7244 0.035 Uiso 1 1 calc R . .
C30 C 0.85316(10) 0.03050(9) 0.5905(3) 0.0366(10) Uani 1 1 d . . .
H30A H 0.8534 0.0319 0.5098 0.044 Uiso 1 1 calc R . .
H30B H 0.8234 0.0109 0.6147 0.044 Uiso 1 1 calc R . .
C31 C 0.88173(13) 0.01406(13) 0.6282(4) 0.0622(13) Uani 1 1 d . . .
H31A H 0.8834 0.0155 0.7088 0.075 Uiso 1 1 calc R . .
H31B H 0.8689 -0.0164 0.6067 0.075 Uiso 1 1 calc R . .
C32 C 0.92558(14) 0.03837(15) 0.5827(5) 0.100(2) Uani 1 1 d . . .
H32A H 0.9431 0.0268 0.6120 0.151 Uiso 1 1 calc R . .
H32B H 0.9384 0.0686 0.6031 0.151 Uiso 1 1 calc R . .
H32C H 0.9243 0.0358 0.5030 0.151 Uiso 1 1 calc R . .
O1 O 0.94914(7) 0.15231(7) 0.6168(2) 0.0349(6) Uani 1 1 d D . .
H1A H 0.9660(9) 0.1562(10) 0.664(2) 0.042 Uiso 1 1 d D . .
O2 O 1.01444(7) 0.32459(7) 0.3418(2) 0.0486(8) Uani 1 1 d . . .
O3 O 0.99111(6) 0.15547(7) 0.8100(2) 0.0355(6) Uani 1 1 d D . .
O4 O 0.89586(7) 0.09102(8) 0.8452(2) 0.0381(7) Uani 1 1 d D . .
H4A H 0.8813(9) 0.0802(10) 0.791(2) 0.046 Uiso 1 1 d D . .
O5 O 0.76589(7) 0.10375(7) 1.1753(2) 0.0438(7) Uani 1 1 d . . .
O6 O 0.86841(6) 0.07299(6) 0.63610(19) 0.0286(6) Uani 1 1 d . . .
S1 S 0.88986(2) 0.12638(2) 0.42852(8) 0.0304(2) Uani 1 1 d . . .
S2 S 1.03139(2) 0.23516(3) 0.67500(8) 0.0374(3) Uani 1 1 d . . .
S3 S 0.94902(3) 0.13573(3) 1.03643(9) 0.0376(3) Uani 1 1 d . . .
S4 S 0.79817(2) 0.04530(2) 0.80105(8) 0.0319(2) Uani 1 1 d . . .
C14 C 1.0287(2) 0.1529(2) 0.8383(10) 0.051(2) Uani 0.826(8) 1 d PDU A 1
H14C H 1.0317 0.1533 0.9187 0.061 Uiso 0.826(8) 1 calc PR A 1
H14D H 1.0546 0.1779 0.8080 0.061 Uiso 0.826(8) 1 calc PR A 1
C15 C 1.0247(2) 0.11264(19) 0.7935(8) 0.074(3) Uani 0.826(8) 1 d PDU A 1
H15C H 1.0526 0.1137 0.8000 0.089 Uiso 0.826(8) 1 calc PR A 1
H15D H 1.0173 0.1104 0.7150 0.089 Uiso 0.826(8) 1 calc PR A 1
C16 C 0.9906(2) 0.07325(19) 0.8526(7) 0.099(3) Uani 0.826(8) 1 d PDU A 1
H16D H 0.9881 0.0474 0.8187 0.148 Uiso 0.826(8) 1 calc PR A 1
H16E H 0.9631 0.0724 0.8478 0.148 Uiso 0.826(8) 1 calc PR A 1
H16F H 0.9987 0.0744 0.9294 0.148 Uiso 0.826(8) 1 calc PR A 1
C14' C 1.0220(13) 0.1452(11) 0.845(5) 0.071(9) Uani 0.174(8) 1 d PDU A 2
H14E H 1.0227 0.1441 0.9253 0.085 Uiso 0.174(8) 1 calc PR A 2
H14F H 1.0508 0.1669 0.8184 0.085 Uiso 0.174(8) 1 calc PR A 2
C15' C 1.0089(13) 0.1005(10) 0.796(4) 0.072(7) Uani 0.174(8) 1 d PDU A 2
H15E H 0.9778 0.0807 0.8054 0.087 Uiso 0.174(8) 1 calc PR A 2
H15F H 1.0156 0.1031 0.7166 0.087 Uiso 0.174(8) 1 calc PR A 2
C16' C 1.0346(8) 0.0840(7) 0.856(3) 0.081(9) Uani 0.174(8) 1 d PDU A 2
H16G H 1.0315 0.0586 0.8189 0.121 Uiso 0.174(8) 1 calc PR A 2
H16H H 1.0239 0.0765 0.9310 0.121 Uiso 0.174(8) 1 calc PR A 2
H16I H 1.0649 0.1063 0.8575 0.121 Uiso 0.174(8) 1 calc PR 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
C1 C6 1.391(4) . ?
C1 C2 1.395(4) . ?
C1 S1 1.786(3) . ?
C2 O1 1.337(4) . ?
C2 C3 1.421(4) . ?
C3 C4 1.378(4) . ?
C3 S2 1.773(3) . ?
C4 C5 1.389(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(4) . ?
C5 C7 1.469(5) . ?
C6 H6 0.9500 . ?
C7 O2 1.213(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.393(4) . ?
C8 C9 1.399(4) . ?
C8 S2 1.783(4) . ?
C9 O3 1.382(3) . ?
C9 C10 1.385(5) . ?
C10 C11 1.392(4) . ?
C10 S3 1.784(3) . ?
C11 C12 1.379(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C17 C22 1.385(5) . ?
C17 C18 1.408(5) . ?
C17 S3 1.776(3) . ?
C18 O4 1.341(4) . ?
C18 C19 1.412(4) . ?
C19 C20 1.375(4) . ?
C19 S4 1.784(3) . ?
C20 C21 1.400(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(4) . ?
C21 C23 1.452(5) . ?
C22 H22 0.9500 . ?
C23 O5 1.206(3) . ?
C23 H23 0.9500 . ?
C24 C29 1.387(4) . ?
C24 C25 1.398(4) . ?
C24 S4 1.787(3) . ?
C25 O6 1.382(3) . ?
C25 C26 1.392(4) . ?
C26 C27 1.390(4) . ?
C26 S1 1.789(3) . ?
C27 C28 1.387(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.375(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 O6 1.455(3) . ?
C30 C31 1.495(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.480(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O1 H1A 0.803(18) . ?
O3 C14' 1.404(16) . ?
O3 C14 1.446(5) . ?
O4 H4A 0.820(18) . ?
C14 C15 1.488(6) . ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?
C15 C16 1.517(9) . ?
C15 H15C 0.9900 . ?
C15 H15D 0.9900 . ?
C16 H16D 0.9800 . ?
C16 H16E 0.9800 . ?
C16 H16F 0.9800 . ?
C14' C15' 1.553(18) . ?
C14' H14E 0.9900 . ?
C14' H14F 0.9900 . ?
C15' C16' 1.519(19) . ?
C15' H15E 0.9900 . ?
C15' H15F 0.9900 . ?
C16' H16G 0.9800 . ?
C16' H16H 0.9800 . ?
C16' H16I 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
C6 C1 C2 119.8(3) . . ?
C6 C1 S1 118.9(3) . . ?
C2 C1 S1 120.9(2) . . ?
O1 C2 C1 117.9(3) . . ?
O1 C2 C3 122.5(3) . . ?
C1 C2 C3 119.5(3) . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 S2 119.9(2) . . ?
C2 C3 S2 120.0(3) . . ?
C3 C4 C5 121.5(3) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 C7 121.6(3) . . ?
C6 C5 C7 119.5(3) . . ?
C1 C6 C5 120.9(3) . . ?
C1 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
O2 C7 C5 124.3(4) . . ?
O2 C7 H7 117.9 . . ?
C5 C7 H7 117.9 . . ?
C13 C8 C9 119.9(3) . . ?
C13 C8 S2 119.8(3) . . ?
C9 C8 S2 120.4(3) . . ?
O3 C9 C10 121.6(3) . . ?
O3 C9 C8 118.4(3) . . ?
C10 C9 C8 119.7(3) . . ?
C9 C10 C11 119.4(3) . . ?
C9 C10 S3 121.8(3) . . ?
C11 C10 S3 118.8(3) . . ?
C12 C11 C10 121.3(4) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 119.4(3) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C12 C13 C8 120.4(3) . . ?
C12 C13 H13 119.8 . . ?
C8 C13 H13 119.8 . . ?
C22 C17 C18 119.4(3) . . ?
C22 C17 S3 119.8(3) . . ?
C18 C17 S3 120.7(3) . . ?
O4 C18 C17 117.0(3) . . ?
O4 C18 C19 123.2(3) . . ?
C17 C18 C19 119.8(3) . . ?
C20 C19 C18 119.4(3) . . ?
C20 C19 S4 119.3(2) . . ?
C18 C19 S4 121.0(3) . . ?
C19 C20 C21 121.6(3) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 H20 119.2 . . ?
C22 C21 C20 118.5(3) . . ?
C22 C21 C23 120.4(3) . . ?
C20 C21 C23 121.0(3) . . ?
C17 C22 C21 121.3(3) . . ?
C17 C22 H22 119.4 . . ?
C21 C22 H22 119.4 . . ?
O5 C23 C21 125.0(3) . . ?
O5 C23 H23 117.5 . . ?
C21 C23 H23 117.5 . . ?
C29 C24 C25 119.4(3) . . ?
C29 C24 S4 120.2(3) . . ?
C25 C24 S4 120.2(2) . . ?
O6 C25 C26 120.5(3) . . ?
O6 C25 C24 119.1(3) . . ?
C26 C25 C24 120.3(3) . . ?
C27 C26 C25 118.8(3) . . ?
C27 C26 S1 119.8(3) . . ?
C25 C26 S1 121.4(2) . . ?
C28 C27 C26 121.2(3) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C29 C28 C27 119.4(3) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C24 120.9(3) . . ?
C28 C29 H29 119.6 . . ?
C24 C29 H29 119.6 . . ?
O6 C30 C31 109.0(3) . . ?
O6 C30 H30A 109.9 . . ?
C31 C30 H30A 109.9 . . ?
O6 C30 H30B 109.9 . . ?
C31 C30 H30B 109.9 . . ?
H30A C30 H30B 108.3 . . ?
C32 C31 C30 113.1(4) . . ?
C32 C31 H31A 109.0 . . ?
C30 C31 H31A 109.0 . . ?
C32 C31 H31B 109.0 . . ?
C30 C31 H31B 109.0 . . ?
H31A C31 H31B 107.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C2 O1 H1A 117(2) . . ?
C9 O3 C14' 120.2(14) . . ?
C9 O3 C14 115.0(3) . . ?
C14' O3 C14 11(3) . . ?
C18 O4 H4A 110(2) . . ?
C25 O6 C30 115.2(2) . . ?
C1 S1 C26 102.09(14) . . ?
C3 S2 C8 103.96(14) . . ?
C17 S3 C10 98.00(14) . . ?
C19 S4 C24 103.72(14) . . ?
O3 C14 C15 109.7(4) . . ?
O3 C14 H14C 109.7 . . ?
C15 C14 H14C 109.7 . . ?
O3 C14 H14D 109.7 . . ?
C15 C14 H14D 109.7 . . ?
H14C C14 H14D 108.2 . . ?
C14 C15 C16 112.0(7) . . ?
C14 C15 H15C 109.2 . . ?
C16 C15 H15C 109.2 . . ?
C14 C15 H15D 109.2 . . ?
C16 C15 H15D 109.2 . . ?
H15C C15 H15D 107.9 . . ?
C15 C16 H16D 109.5 . . ?
C15 C16 H16E 109.5 . . ?
H16D C16 H16E 109.5 . . ?
C15 C16 H16F 109.5 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?
O3 C14' C15' 106.7(17) . . ?
O3 C14' H14E 110.4 . . ?
C15' C14' H14E 110.4 . . ?
O3 C14' H14F 110.4 . . ?
C15' C14' H14F 110.4 . . ?
H14E C14' H14F 108.6 . . ?
C16' C15' C14' 106.7(16) . . ?
C16' C15' H15E 110.4 . . ?
C14' C15' H15E 110.4 . . ?
C16' C15' H15F 110.4 . . ?
C14' C15' H15F 110.4 . . ?
H15E C15' H15F 108.6 . . ?
C15' C16' H16G 109.5 . . ?
C15' C16' H16H 109.5 . . ?
H16G C16' H16H 109.5 . . ?
C15' C16' H16I 109.5 . . ?
H16G C16' H16I 109.5 . . ?
H16H C16' H16I 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1056805'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H28 O7 S4'
_chemical_formula_weight         664.79

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

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R -3'
_symmetry_space_group_name_Hall  '-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                   37.498(5)
_cell_length_b                   37.498(5)
_cell_length_c                   11.9203(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     14515(3)
_cell_formula_units_Z            18
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9147
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      24.11

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6228
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9349
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(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            39803
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.69
_reflns_number_total             6121
_reflns_number_gt                3853
_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)+(0.0842P)²+34.5835P] 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         6121
_refine_ls_number_parameters     505
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.2095
_refine_ls_wR_factor_gt          0.1616
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.128
_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
C1 C 0.55905(14) 0.10449(16) 0.3657(3) 0.0822(13) Uani 1 1 d . . .
C2 C 0.53288(14) 0.07526(15) 0.4404(3) 0.0801(12) Uani 1 1 d . . .
H2 H 0.5436 0.0711 0.5063 0.096 Uiso 1 1 calc R . .
C3 C 0.49102(14) 0.05180(14) 0.4204(3) 0.0746(11) Uani 1 1 d D H .
C4 C 0.47505(14) 0.05922(15) 0.3218(3) 0.0754(11) Uani 1 1 d . . .
H4 H 0.4469 0.0440 0.3078 0.090 Uiso 1 1 calc R . .
C5 C 0.50021(14) 0.08840(15) 0.2465(3) 0.0757(12) Uani 1 1 d . . .
C6 C 0.54282(15) 0.11160(16) 0.2662(3) 0.0807(12) Uani 1 1 d . . .
C7 C 0.46418(18) 0.02056(17) 0.5002(4) 0.0911(14) Uani 1 1 d D . .
H7A H 0.4364 0.0091 0.4833 0.109 Uiso 0.31 1 calc PR A 2
H7 H 0.4757 0.0187 0.5674 0.109 Uiso 0.69 1 d PR A 1
C8 C 0.48937(14) 0.07596(17) 0.0180(3) 0.0772(12) Uani 1 1 d D . .
C9 C 0.46519(15) 0.03440(19) 0.0041(4) 0.0910(14) Uani 1 1 d D . .
H9 H 0.4439 0.0190 0.0540 0.109 Uiso 1 1 calc R . .
C10 C 0.47264(16) 0.01541(17) -0.0851(5) 0.0967(16) Uani 1 1 d D L .
H10 H 0.4560 -0.0140 -0.0943 0.116 Uiso 0.61 1 d PR B 2
C11 C 0.50378(16) 0.03748(19) -0.1602(4) 0.0892(14) Uani 1 1 d D . .
H11 H 0.5081 0.0241 -0.2199 0.107 Uiso 1 1 calc R . .
C12 C 0.52835(14) 0.07904(17) -0.1474(3) 0.0788(12) Uani 1 1 d D . .
C13 C 0.52122(13) 0.09869(15) -0.0578(3) 0.0725(11) Uani 1 1 d D C .
C15' C 0.5425(8) 0.1683(5) -0.1069(16) 0.114(9) Uani 0.43 1 d PD C 2
H15A H 0.5507 0.1674 -0.1835 0.137 Uiso 0.43 1 calc PR C 2
H15B H 0.5138 0.1613 -0.1074 0.137 Uiso 0.43 1 calc PR C 2
C16' C 0.5670(14) 0.2077(7) -0.062(4) 0.182(12) Uani 0.43 1 d P C 2
H16A H 0.5935 0.2162 -0.0966 0.218 Uiso 0.43 1 calc PR C 2
H16B H 0.5566 0.2234 -0.1013 0.218 Uiso 0.43 1 calc PR C 2
C17' C 0.5767(11) 0.2247(7) 0.027(2) 0.182(11) Uani 0.43 1 d PD C 2
H17A H 0.6039 0.2303 0.0459 0.273 Uiso 0.43 1 calc PR C 2
H17B H 0.5576 0.2074 0.0831 0.273 Uiso 0.43 1 calc PR C 2
H17C H 0.5765 0.2502 0.0228 0.273 Uiso 0.43 1 calc PR C 2
C18 C 0.60659(13) 0.09599(16) -0.2064(3) 0.0812(12) Uani 1 1 d . . .
C19 C 0.61575(14) 0.07159(17) -0.2730(4) 0.0912(14) Uani 1 1 d . . .
H19 H 0.5996 0.0588 -0.3357 0.109 Uiso 1 1 calc R . .
C20 C 0.64867(15) 0.06570(16) -0.2481(4) 0.0889(13) Uani 1 1 d D J .
C21 C 0.67285(14) 0.08552(16) -0.1550(4) 0.0874(13) Uani 1 1 d . . .
H21 H 0.6949 0.0817 -0.1374 0.105 Uiso 1 1 calc R . .
C22 C 0.66491(12) 0.11063(15) -0.0883(3) 0.0761(12) Uani 1 1 d . . .
C23 C 0.63147(12) 0.11597(15) -0.1133(3) 0.0742(11) Uani 1 1 d . . .
C24 C 0.6578(2) 0.0401(2) -0.3215(6) 0.126(2) Uani 1 1 d D . .
H24 H 0.6408 0.0285 -0.3834 0.151 Uiso 0.78 1 calc PR D 1
H24A H 0.6814 0.0367 -0.3055 0.151 Uiso 0.22 1 d PR D 2
C25 C 0.66990(12) 0.11386(17) 0.1427(4) 0.0818(13) Uani 1 1 d . . .
C26 C 0.66433(14) 0.07587(18) 0.1709(4) 0.0914(14) Uani 1 1 d . M .
H26 H 0.6747 0.0632 0.1244 0.110 Uiso 1 1 calc R . .
C27 C 0.64377(16) 0.05658(19) 0.2665(5) 0.1009(16) Uani 1 1 d D . .
H27 H 0.6399 0.0308 0.2848 0.121 Uiso 0.39 1 calc PR E 1
C28 C 0.62863(15) 0.0753(2) 0.3361(4) 0.1021(17) Uani 1 1 d . M .
H28 H 0.6153 0.0624 0.4023 0.122 Uiso 1 1 calc R . .
C29 C 0.63294(13) 0.11274(18) 0.3087(4) 0.0867(14) Uani 1 1 d . . .
C30 C 0.65407(12) 0.13219(16) 0.2118(3) 0.0790(12) Uani 1 1 d D F .
C32' C 0.6838(13) 0.2044(6) 0.237(4) 0.133(16) Uani 0.34 1 d PD F 2
H32A H 0.7113 0.2079 0.2341 0.160 Uiso 0.34 1 calc PR F 2
H32B H 0.6758 0.2020 0.3157 0.160 Uiso 0.34 1 calc PR F 2
C33' C 0.684(2) 0.2405(18) 0.186(7) 0.199(19) Uani 0.34 1 d P F 2
H33A H 0.6950 0.2431 0.1109 0.239 Uiso 0.34 1 calc PR F 2
H33B H 0.6552 0.2328 0.1769 0.239 Uiso 0.34 1 calc PR F 2
C34' C 0.7026(10) 0.2778(7) 0.229(3) 0.199(13) Uani 0.34 1 d PD F 2
H34A H 0.7311 0.2867 0.2413 0.299 Uiso 0.34 1 calc PR F 2
H34B H 0.6899 0.2776 0.2993 0.299 Uiso 0.34 1 calc PR F 2
H34C H 0.7003 0.2965 0.1783 0.299 Uiso 0.34 1 calc PR F 2
O1 O 0.56775(10) 0.14010(12) 0.1943(3) 0.1014(11) Uani 1 1 d . . .
H1 H 0.5914 0.1514 0.2186 0.152 Uiso 0.50 1 calc PR G 1
H1' H 0.5543 0.1411 0.1413 0.152 Uiso 0.50 1 d PR G 2
O2 O 0.42930(19) -0.00257(18) 0.4859(5) 0.1153(18) Uani 0.69 1 d PD H 1
O3 O 0.54738(10) 0.13949(11) -0.0393(3) 0.0900(9) Uani 1 1 d D . .
O5 O 0.62416(10) 0.14093(11) -0.0499(3) 0.0906(9) Uani 1 1 d . . .
H5 H 0.6440 0.1545 -0.0089 0.136 Uiso 0.50 1 calc PR I 1
H5' H 0.6038 0.1412 -0.0735 0.136 Uiso 0.50 1 d PR I 2
O6 O 0.68542(19) 0.0326(2) -0.3096(6) 0.147(2) Uani 0.78 1 d PD J 1
O7 O 0.65566(10) 0.16792(12) 0.1785(3) 0.1020(10) Uani 1 1 d D . .
O2' O 0.4704(4) 0.0066(4) 0.5826(8) 0.106(3) Uani 0.31 1 d PD H 2
O6' O 0.6362(8) 0.0241(10) -0.4007(19) 0.210(15) Uani 0.22 1 d PD J 2
S1 S 0.47828(4) 0.09994(5) 0.13009(10) 0.0995(5) Uani 1 1 d . . .
S2 S 0.56739(4) 0.10667(5) -0.24838(9) 0.0994(5) Uani 1 1 d . . .
S3 S 0.69953(3) 0.13949(5) 0.02125(10) 0.0978(5) Uani 1 1 d . . .
S4 S 0.61185(4) 0.13524(6) 0.39891(11) 0.1132(6) Uani 1 1 d . M .
C15 C 0.5322(6) 0.1663(4) -0.0716(14) 0.104(6) Uani 0.57 1 d PD C 1
H15C H 0.5042 0.1546 -0.0449 0.125 Uiso 0.57 1 calc PR C 1
H15D H 0.5315 0.1671 -0.1528 0.125 Uiso 0.57 1 calc PR C 1
C16 C 0.5566(10) 0.2095(5) -0.029(3) 0.36(4) Uani 0.57 1 d PD C 1
H16C H 0.5399 0.2225 -0.0343 0.433 Uiso 0.57 1 calc PR C 1
H16D H 0.5632 0.2090 0.0492 0.433 Uiso 0.57 1 calc PR C 1
C17 C 0.5954(10) 0.2346(9) -0.093(3) 0.36(2) Uani 0.57 1 d PD C 1
H17D H 0.6055 0.2171 -0.1198 0.541 Uiso 0.57 1 calc PR C 1
H17E H 0.6157 0.2554 -0.0448 0.541 Uiso 0.57 1 calc PR C 1
H17F H 0.5902 0.2475 -0.1556 0.541 Uiso 0.57 1 calc PR C 1
C32 C 0.6927(5) 0.2053(3) 0.204(2) 0.133(8) Uani 0.66 1 d PD F 1
H32C H 0.7164 0.2034 0.1797 0.160 Uiso 0.66 1 calc PR F 1
H32D H 0.6948 0.2100 0.2845 0.160 Uiso 0.66 1 calc PR F 1
C33 C 0.6918(11) 0.2408(7) 0.144(3) 0.31(3) Uani 0.66 1 d PD F 1
H33C H 0.7188 0.2653 0.1459 0.374 Uiso 0.66 1 calc PR F 1
H33D H 0.6838 0.2336 0.0661 0.374 Uiso 0.66 1 calc PR F 1
C34 C 0.6612(7) 0.2482(7) 0.203(3) 0.31(2) Uani 0.66 1 d PD F 1
H34D H 0.6346 0.2238 0.2007 0.468 Uiso 0.66 1 calc PR F 1
H34E H 0.6598 0.2705 0.1677 0.468 Uiso 0.66 1 calc PR F 1
H34F H 0.6694 0.2553 0.2802 0.468 Uiso 0.66 1 calc PR F 1
C14 C 0.4482(3) -0.0280(3) -0.1023(10) 0.151(4) Uani 0.75 1 d PD . .
H14 H 0.4555 -0.0380 -0.1675 0.181 Uiso 0.38 1 d PR K 3
H14A H 0.4273 -0.0402 -0.0456 0.181 Uiso 0.38 1 d PR K 2
O4A O 0.4462(5) -0.0507(5) -0.1589(15) 0.168(7) Uani 0.38 1 d PD L 2
O4 O 0.4219(3) -0.0523(4) -0.0525(12) 0.162(7) Uani 0.38 1 d PD L 3
C14B C 0.6390(7) 0.0182(5) 0.2976(18) 0.117(8) Uani 0.25 1 d PD M 3
H14B H 0.6452 0.0028 0.2483 0.141 Uiso 0.25 1 calc PR M 3
O4B O 0.6266(9) 0.0062(8) 0.390(2) 0.209(13) Uani 0.25 1 d PD M 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
C1 C2 1.372(6) . ?
C1 C6 1.418(6) . ?
C1 S4 1.767(5) . ?
C2 C3 1.383(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.409(6) . ?
C3 C7 1.452(6) . ?
C4 C5 1.364(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.405(6) . ?
C5 S1 1.773(4) . ?
C6 O1 1.324(5) . ?
C7 O2 1.165(6) . ?
C7 O2' 1.189(8) . ?
C7 H7A 0.9300 . ?
C7 H7 0.9300 . ?
C8 C9 1.366(7) . ?
C8 C13 1.397(6) . ?
C8 S1 1.772(5) . ?
C9 C10 1.383(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.373(8) . ?
C10 C14 1.427(8) . ?
C10 H10 0.9645 . ?
C11 C12 1.366(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.397(6) . ?
C12 S2 1.775(5) . ?
C13 O3 1.361(5) . ?
C15' C16' 1.40(3) . ?
C15' O3 1.431(9) . ?
C15' H15A 0.9700 . ?
C15' H15B 0.9700 . ?
C16' C17' 1.20(5) . ?
C16' H16A 0.9700 . ?
C16' H16B 0.9700 . ?
C17' H17A 0.9600 . ?
C17' H17B 0.9600 . ?
C17' H17C 0.9600 . ?
C18 C19 1.378(7) . ?
C18 C23 1.401(6) . ?
C18 S2 1.778(5) . ?
C19 C20 1.390(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.391(7) . ?
C20 C24 1.460(6) . ?
C21 C22 1.374(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.397(6) . ?
C22 S3 1.777(4) . ?
C23 O5 1.335(5) . ?
C24 O6' 1.194(10) . ?
C24 O6 1.208(6) . ?
C24 H24 0.9300 . ?
C24 H24A 0.9733 . ?
C25 C26 1.374(7) . ?
C25 C30 1.383(7) . ?
C25 S3 1.785(5) . ?
C26 C27 1.363(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.379(8) . ?
C27 C14B 1.411(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.370(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.384(6) . ?
C29 S4 1.778(5) . ?
C30 O7 1.370(6) . ?
C32' O7 1.427(10) . ?
C32' C33' 1.49(4) . ?
C32' H32A 0.9700 . ?
C32' H32B 0.9700 . ?
C33' C34' 1.32(6) . ?
C33' H33A 0.9700 . ?
C33' H33B 0.9700 . ?
C34' H34A 0.9600 . ?
C34' H34B 0.9600 . ?
C34' H34C 0.9600 . ?
O1 H1 0.8200 . ?
O1 H1' 0.8201 . ?
O3 C15 1.432(9) . ?
O5 H5 0.8200 . ?
O5 H5' 0.8200 . ?
O6 H24A 0.2674 . ?
O7 C32 1.428(9) . ?
O2' H7 0.4321 . ?
C15 C16 1.495(10) . ?
C15 H15C 0.9700 . ?
C15 H15D 0.9700 . ?
C16 C17 1.488(11) . ?
C16 H16C 0.9700 . ?
C16 H16D 0.9700 . ?
C17 H17D 0.9600 . ?
C17 H17E 0.9600 . ?
C17 H17F 0.9600 . ?
C32 C33 1.527(11) . ?
C32 H32C 0.9700 . ?
C32 H32D 0.9700 . ?
C33 C34 1.490(11) . ?
C33 H33C 0.9700 . ?
C33 H33D 0.9700 . ?
C34 H34D 0.9600 . ?
C34 H34E 0.9600 . ?
C34 H34F 0.9600 . ?
C14 O4A 1.060(9) . ?
C14 O4 1.122(9) . ?
C14 H10 0.4640 . ?
C14 H14 0.9601 . ?
C14 H14A 0.9600 . ?
C14B O4B 1.198(10) . ?
C14B H14B 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 119.4(4) . . ?
C2 C1 S4 119.8(3) . . ?
C6 C1 S4 120.7(4) . . ?
C1 C2 C3 121.9(4) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 H2 119.1 . . ?
C2 C3 C4 118.5(4) . . ?
C2 C3 C7 120.6(4) . . ?
C4 C3 C7 120.9(4) . . ?
C5 C4 C3 121.0(4) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 S1 119.4(3) . . ?
C6 C5 S1 120.1(4) . . ?
O1 C6 C5 121.1(4) . . ?
O1 C6 C1 119.8(4) . . ?
C5 C6 C1 119.0(4) . . ?
O2 C7 O2' 100.8(8) . . ?
O2 C7 C3 124.9(5) . . ?
O2' C7 C3 133.3(8) . . ?
O2 C7 H7A 16.7 . . ?
O2' C7 H7A 113.3 . . ?
C3 C7 H7A 113.3 . . ?
O2 C7 H7 117.5 . . ?
O2' C7 H7 18.9 . . ?
C3 C7 H7 117.7 . . ?
H7A C7 H7 127.4 . . ?
C9 C8 C13 119.6(4) . . ?
C9 C8 S1 118.7(4) . . ?
C13 C8 S1 121.6(4) . . ?
C8 C9 C10 119.4(5) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C11 C10 C9 121.4(5) . . ?
C11 C10 C14 117.4(8) . . ?
C9 C10 C14 121.2(8) . . ?
C11 C10 H10 119.0 . . ?
C9 C10 H10 119.6 . . ?
C14 C10 H10 1.7 . . ?
C12 C11 C10 120.0(5) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 119.3(5) . . ?
C11 C12 S2 118.6(4) . . ?
C13 C12 S2 122.0(4) . . ?
O3 C13 C12 119.8(4) . . ?
O3 C13 C8 119.8(4) . . ?
C12 C13 C8 120.2(5) . . ?
C16' C15' O3 108.6(16) . . ?
C16' C15' H15A 110.0 . . ?
O3 C15' H15A 110.0 . . ?
C16' C15' H15B 110.0 . . ?
O3 C15' H15B 110.0 . . ?
H15A C15' H15B 108.3 . . ?
C17' C16' C15' 140(5) . . ?
C17' C16' H16A 102.1 . . ?
C15' C16' H16A 102.1 . . ?
C17' C16' H16B 102.1 . . ?
C15' C16' H16B 102.1 . . ?
H16A C16' H16B 104.8 . . ?
C16' C17' H17A 109.5 . . ?
C16' C17' H17B 109.5 . . ?
H17A C17' H17B 109.5 . . ?
C16' C17' H17C 109.5 . . ?
H17A C17' H17C 109.5 . . ?
H17B C17' H17C 109.5 . . ?
C19 C18 C23 119.4(4) . . ?
C19 C18 S2 119.8(3) . . ?
C23 C18 S2 120.4(4) . . ?
C18 C19 C20 121.2(4) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 H19 119.4 . . ?
C19 C20 C21 118.6(5) . . ?
C19 C20 C24 119.8(5) . . ?
C21 C20 C24 121.6(5) . . ?
C22 C21 C20 121.4(4) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 119.5(4) . . ?
C21 C22 S3 120.0(3) . . ?
C23 C22 S3 120.3(4) . . ?
O5 C23 C22 119.5(4) . . ?
O5 C23 C18 120.6(4) . . ?
C22 C23 C18 119.9(4) . . ?
O6' C24 O6 115.0(14) . . ?
O6' C24 C20 118.6(12) . . ?
O6 C24 C20 126.4(7) . . ?
O6' C24 H24 2.0 . . ?
O6 C24 H24 116.8 . . ?
C20 C24 H24 116.8 . . ?
O6' C24 H24A 121.6 . . ?
O6 C24 H24A 6.8 . . ?
C20 C24 H24A 119.8 . . ?
H24 C24 H24A 123.4 . . ?
C26 C25 C30 119.3(4) . . ?
C26 C25 S3 119.2(4) . . ?
C30 C25 S3 121.5(4) . . ?
C27 C26 C25 120.4(5) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C26 C27 C28 120.1(6) . . ?
C26 C27 C14B 120.7(10) . . ?
C28 C27 C14B 119.2(10) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C14B C27 H27 2.2 . . ?
C29 C28 C27 120.7(5) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 118.8(5) . . ?
C28 C29 S4 119.3(4) . . ?
C30 C29 S4 121.9(5) . . ?
O7 C30 C25 119.6(4) . . ?
O7 C30 C29 119.4(5) . . ?
C25 C30 C29 120.7(5) . . ?
O7 C32' C33' 109(3) . . ?
O7 C32' H32A 109.8 . . ?
C33' C32' H32A 109.8 . . ?
O7 C32' H32B 109.8 . . ?
C33' C32' H32B 109.8 . . ?
H32A C32' H32B 108.2 . . ?
C34' C33' C32' 124(5) . . ?
C34' C33' H33A 106.2 . . ?
C32' C33' H33A 106.2 . . ?
C34' C33' H33B 106.2 . . ?
C32' C33' H33B 106.2 . . ?
H33A C33' H33B 106.4 . . ?
C33' C34' H34A 109.5 . . ?
C33' C34' H34B 109.5 . . ?
H34A C34' H34B 109.5 . . ?
C33' C34' H34C 109.5 . . ?
H34A C34' H34C 109.5 . . ?
H34B C34' H34C 109.5 . . ?
C6 O1 H1 109.5 . . ?
C6 O1 H1' 109.6 . . ?
H1 O1 H1' 140.9 . . ?
C13 O3 C15' 117.7(10) . . ?
C13 O3 C15 115.4(7) . . ?
C15' O3 C15 22.1(14) . . ?
C23 O5 H5 109.5 . . ?
C23 O5 H5' 109.6 . . ?
H5 O5 H5' 139.3 . . ?
C24 O6 H24A 25.5 . . ?
C30 O7 C32' 116.3(13) . . ?
C30 O7 C32 116.3(8) . . ?
C32' O7 C32 20(3) . . ?
C7 O2' H7 44.3 . . ?
C8 S1 C5 102.18(18) . . ?
C12 S2 C18 102.20(19) . . ?
C22 S3 C25 101.52(19) . . ?
C1 S4 C29 100.0(2) . . ?
O3 C15 C16 115.4(15) . . ?
O3 C15 H15C 108.4 . . ?
C16 C15 H15C 108.4 . . ?
O3 C15 H15D 108.4 . . ?
C16 C15 H15D 108.4 . . ?
H15C C15 H15D 107.5 . . ?
C17 C16 C15 112.7(15) . . ?
C17 C16 H16C 109.0 . . ?
C15 C16 H16C 109.0 . . ?
C17 C16 H16D 109.0 . . ?
C15 C16 H16D 109.0 . . ?
H16C C16 H16D 107.8 . . ?
O7 C32 C33 108.6(15) . . ?
O7 C32 H32C 110.0 . . ?
C33 C32 H32C 110.0 . . ?
O7 C32 H32D 110.0 . . ?
C33 C32 H32D 110.0 . . ?
H32C C32 H32D 108.3 . . ?
C34 C33 C32 107.1(14) . . ?
C34 C33 H33C 110.3 . . ?
C32 C33 H33C 110.3 . . ?
C34 C33 H33D 110.3 . . ?
C32 C33 H33D 110.3 . . ?
H33C C33 H33D 108.5 . . ?
O4A C14 O4 90.1(15) . . ?
O4A C14 C10 139.1(18) . . ?
O4 C14 C10 130.9(16) . . ?
O4A C14 H10 142.2 . . ?
O4 C14 H10 127.6 . . ?
C10 C14 H10 3.6 . . ?
O4A C14 H14 24.5 . . ?
O4 C14 H14 114.6 . . ?
C10 C14 H14 114.6 . . ?
H10 C14 H14 117.8 . . ?
O4A C14 H14A 110.5 . . ?
O4 C14 H14A 20.4 . . ?
C10 C14 H14A 110.5 . . ?
H10 C14 H14A 107.3 . . ?
H14 C14 H14A 134.9 . . ?
C14 O4A H10 11.3 . . ?
C14 O4A H14 64.9 . . ?
H10 O4A H14 53.7 . . ?
C14 O4 H10 14.7 . . ?
C14 O4 H14A 56.5 . . ?
H10 O4 H14A 41.9 . . ?
O4B C14B C27 116.9(15) . . ?
O4B C14B H14B 121.6 . . ?
C27 C14B H14B 121.6 . . ?

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
C6 C1 C2 C3 1.3(7) . . . . ?
S4 C1 C2 C3 176.9(3) . . . . ?
C1 C2 C3 C4 -1.8(6) . . . . ?
C1 C2 C3 C7 178.9(4) . . . . ?
C2 C3 C4 C5 1.0(6) . . . . ?
C7 C3 C4 C5 -179.7(4) . . . . ?
C3 C4 C5 C6 0.2(6) . . . . ?
C3 C4 C5 S1 -174.3(3) . . . . ?
C4 C5 C6 O1 -179.9(4) . . . . ?
S1 C5 C6 O1 -5.4(6) . . . . ?
C4 C5 C6 C1 -0.6(6) . . . . ?
S1 C5 C6 C1 173.8(3) . . . . ?
C2 C1 C6 O1 179.2(4) . . . . ?
S4 C1 C6 O1 3.6(6) . . . . ?
C2 C1 C6 C5 -0.1(7) . . . . ?
S4 C1 C6 C5 -175.7(3) . . . . ?
C2 C3 C7 O2 -173.8(6) . . . . ?
C4 C3 C7 O2 6.9(8) . . . . ?
C2 C3 C7 O2' -7.6(12) . . . . ?
C4 C3 C7 O2' 173.1(10) . . . . ?
C13 C8 C9 C10 0.1(3) . . . . ?
S1 C8 C9 C10 178.0(2) . . . . ?
C8 C9 C10 C11 -0.25(18) . . . . ?
C8 C9 C10 C14 179.7(3) . . . . ?
C9 C10 C11 C12 0.46(18) . . . . ?
C14 C10 C11 C12 -179.5(3) . . . . ?
C10 C11 C12 C13 -0.5(4) . . . . ?
C10 C11 C12 S2 -178.4(2) . . . . ?
C11 C12 C13 O3 175.0(3) . . . . ?
S2 C12 C13 O3 -7.2(4) . . . . ?
C11 C12 C13 C8 0.3(4) . . . . ?
S2 C12 C13 C8 178.1(2) . . . . ?
C9 C8 C13 O3 -174.8(3) . . . . ?
S1 C8 C13 O3 7.3(4) . . . . ?
C9 C8 C13 C12 -0.1(4) . . . . ?
S1 C8 C13 C12 -178.0(2) . . . . ?
O3 C15' C16' C17' -41(8) . . . . ?
C23 C18 C19 C20 1.4(7) . . . . ?
S2 C18 C19 C20 174.0(4) . . . . ?
C18 C19 C20 C21 -1.0(8) . . . . ?
C18 C19 C20 C24 -179.1(5) . . . . ?
C19 C20 C21 C22 -0.3(7) . . . . ?
C24 C20 C21 C22 177.9(5) . . . . ?
C20 C21 C22 C23 1.0(7) . . . . ?
C20 C21 C22 S3 -173.6(4) . . . . ?
C21 C22 C23 O5 -178.8(4) . . . . ?
S3 C22 C23 O5 -4.3(6) . . . . ?
C21 C22 C23 C18 -0.5(6) . . . . ?
S3 C22 C23 C18 174.0(3) . . . . ?
C19 C18 C23 O5 177.6(4) . . . . ?
S2 C18 C23 O5 5.1(6) . . . . ?
C19 C18 C23 C22 -0.7(7) . . . . ?
S2 C18 C23 C22 -173.2(3) . . . . ?
C19 C20 C24 O6' -1(2) . . . . ?
C21 C20 C24 O6' -179(2) . . . . ?
C19 C20 C24 O6 179.9(8) . . . . ?
C21 C20 C24 O6 1.8(11) . . . . ?
C30 C25 C26 C27 -0.6(7) . . . . ?
S3 C25 C26 C27 176.4(4) . . . . ?
C25 C26 C27 C28 -0.4(7) . . . . ?
C25 C26 C27 C14B -178.1(12) . . . . ?
C26 C27 C28 C29 1.9(8) . . . . ?
C14B C27 C28 C29 179.6(12) . . . . ?
C27 C28 C29 C30 -2.3(7) . . . . ?
C27 C28 C29 S4 178.4(4) . . . . ?
C26 C25 C30 O7 -173.1(4) . . . . ?
S3 C25 C30 O7 9.9(5) . . . . ?
C26 C25 C30 C29 0.2(6) . . . . ?
S3 C25 C30 C29 -176.7(3) . . . . ?
C28 C29 C30 O7 174.6(4) . . . . ?
S4 C29 C30 O7 -6.1(5) . . . . ?
C28 C29 C30 C25 1.2(6) . . . . ?
S4 C29 C30 C25 -179.5(3) . . . . ?
O7 C32' C33' C34' 171(6) . . . . ?
C12 C13 O3 C15' 80.0(12) . . . . ?
C8 C13 O3 C15' -105.2(12) . . . . ?
C12 C13 O3 C15 104.7(9) . . . . ?
C8 C13 O3 C15 -80.5(9) . . . . ?
C16' C15' O3 C13 170(3) . . . . ?
C16' C15' O3 C15 80(4) . . . . ?
C25 C30 O7 C32' -109(3) . . . . ?
C29 C30 O7 C32' 77(3) . . . . ?
C25 C30 O7 C32 -86.2(13) . . . . ?
C29 C30 O7 C32 100.4(13) . . . . ?
C33' C32' O7 C30 176(4) . . . . ?
C33' C32' O7 C32 81(7) . . . . ?
C9 C8 S1 C5 79.2(3) . . . . ?
C13 C8 S1 C5 -102.9(3) . . . . ?
C4 C5 S1 C8 -105.6(4) . . . . ?
C6 C5 S1 C8 79.9(4) . . . . ?
C11 C12 S2 C18 -78.9(3) . . . . ?
C13 C12 S2 C18 103.2(3) . . . . ?
C19 C18 S2 C12 111.1(4) . . . . ?
C23 C18 S2 C12 -76.4(4) . . . . ?
C21 C22 S3 C25 -110.0(4) . . . . ?
C23 C22 S3 C25 75.5(4) . . . . ?
C26 C25 S3 C22 74.0(4) . . . . ?
C30 C25 S3 C22 -109.0(4) . . . . ?
C2 C1 S4 C29 106.1(4) . . . . ?
C6 C1 S4 C29 -78.4(4) . . . . ?
C28 C29 S4 C1 -75.1(4) . . . . ?
C30 C29 S4 C1 105.6(4) . . . . ?
C13 O3 C15 C16 167.3(14) . . . . ?
C15' O3 C15 C16 -91(4) . . . . ?
O3 C15 C16 C17 77(4) . . . . ?
C30 O7 C32 C33 170.5(14) . . . . ?
C32' O7 C32 C33 -94(5) . . . . ?
O7 C32 C33 C34 73(3) . . . . ?
C11 C10 C14 O4A 0.4(17) . . . . ?
C9 C10 C14 O4A -179.5(16) . . . . ?
C11 C10 C14 O4 178.6(6) . . . . ?
C9 C10 C14 O4 -1.4(8) . . . . ?
C26 C27 C14B O4B 168(2) . . . . ?
C28 C27 C14B O4B -9(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5' S2 0.82 2.47 3.008(3) 123.8 .
O5 H5' O3 0.82 2.12 2.855(4) 148.7 .
O5 H5 S3 0.82 2.44 2.977(3) 123.9 .
O5 H5 O7 0.82 2.28 2.938(5) 137.2 .
O1 H1' S1 0.82 2.48 3.009(4) 123.6 .
O1 H1' O3 0.82 2.16 2.884(4) 146.4 .
O1 H1 S4 0.82 2.46 3.003(4) 124.8 .
O1 H1 O7 0.82 2.22 2.924(5) 144.0 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.69
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.051
####################################################################### 
# 
# 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_12.CHCl3
_database_code_depnum_ccdc_archive 'CCDC 1056806'
_audit_update_record             
;
2015-08-27 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '6 (C32 H26 N2 O4 S4).10 (C H Cl3)'
_chemical_formula_sum            'C202 H166 Cl30 N12 O24 S24'
_chemical_formula_weight         4978.40

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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, -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'

_cell_length_a                   23.994(6)
_cell_length_b                   23.994(6)
_cell_length_c                   11.648(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5807(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2962
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      19.11

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             2548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    0.629
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9628
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_process_details   'SADABS, Sheldrick,2008'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23834
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.697
_diffrn_reflns_theta_max         25.004
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             3427
_reflns_number_gt                1552
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

EQIV $2 -x+y+1, -x+1, z 
EQIV $1 -y+1, x-y, z 
SIMU 0.02 0.05 2.0 C13, C14, C15 
DFIX 1.52 0.02 C14 C15 
DFIX 2.85 0.02 Cl3 Cl3_$1, Cl3 Cl3_$2 
DFIX 2.85 0.015 Cl1 Cl2, Cl1 Cl2', Cl2 Cl2' 
DFIX 1.75 0.02 C18 Cl3, C18 Cl3' 
DFIX 1.75 0.01 C17 Cl1, C17 Cl2' 
DFIX 1.75 0.005 C17 Cl2 
DFIX 2.50 0.03 C13 C15 
ISOR 0.02 Cl2, Cl2', Cl3, Cl3', C14, C15, C17 
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.2000P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3427
_refine_ls_number_parameters     234
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.2083
_refine_ls_R_factor_gt           0.1262
_refine_ls_wR_factor_ref         0.4332
_refine_ls_wR_factor_gt          0.3612
_refine_ls_goodness_of_fit_ref   1.375
_refine_ls_restrained_S_all      1.528
_refine_ls_shift/su_max          0.004
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.27498(14) 0.30546(14) 0.42188(18) 0.0944(10) Uani 1 1 d . . . . .
S2 S 0.20602(14) 0.39281(16) 0.8063(2) 0.0986(11) Uani 1 1 d . . . . .
O1 O 0.2047(3) 0.2951(3) 0.6447(5) 0.0869(19) Uani 1 1 d . . . . .
O2 O 0.2407(4) 0.2907(3) 0.8736(5) 0.0895(19) Uani 1 1 d . . . . .
H2 H 0.2042 0.2812 0.8539 0.134 Uiso 1 1 calc R U . . .
N1 N 0.3777(8) 0.5473(7) 1.2163(12) 0.170(5) Uani 1 1 d . . . . .
C1 C 0.2464(4) 0.3567(5) 0.6122(7) 0.071(2) Uani 1 1 d . . . . .
C2 C 0.2836(4) 0.3694(5) 0.5145(7) 0.075(2) Uani 1 1 d . . . . .
C3 C 0.3270(5) 0.4317(5) 0.4869(7) 0.084(3) Uani 1 1 d . . . . .
H3 H 0.3510 0.4399 0.4199 0.101 Uiso 1 1 calc R U . . .
C4 C 0.3366(6) 0.4827(6) 0.5538(9) 0.100(3) Uani 1 1 d . . . . .
H4 H 0.3670 0.5245 0.5329 0.120 Uiso 1 1 calc R U . . .
C5 C 0.3011(5) 0.4714(5) 0.6518(8) 0.088(3) Uani 1 1 d . . . . .
H5 H 0.3066 0.5056 0.6977 0.106 Uiso 1 1 calc R U . . .
C6 C 0.2563(4) 0.4079(5) 0.6824(7) 0.075(2) Uani 1 1 d . . . . .
C7 C 0.2649(4) 0.3419(5) 0.9394(7) 0.078(3) Uani 1 1 d . . . . .
C8 C 0.2569(5) 0.3961(5) 0.9183(7) 0.081(3) Uani 1 1 d . . . . .
C9 C 0.2851(5) 0.4493(6) 0.9914(8) 0.089(3) Uani 1 1 d . . . . .
H9 H 0.2807 0.4850 0.9770 0.107 Uiso 1 1 calc R U . . .
C10 C 0.3204(5) 0.4482(6) 1.0876(7) 0.089(3) Uani 1 1 d . . . . .
C11 C 0.3253(5) 0.3954(5) 1.1103(7) 0.081(3) Uani 1 1 d . . . . .
H11 H 0.3467 0.3950 1.1766 0.098 Uiso 1 1 calc R U . . .
C12 C 0.3007(5) 0.3436(5) 1.0411(7) 0.084(3) Uani 1 1 d . . . . .
C13 C 0.1400(5) 0.2698(6) 0.6012(13) 0.132(5) Uani 1 1 d D U . . .
H13A H 0.1380 0.2603 0.5199 0.159 Uiso 1 1 calc R U . . .
H13B H 0.1250 0.3002 0.6132 0.159 Uiso 1 1 calc R U . . .
C14 C 0.0972(8) 0.2048(9) 0.6744(18) 0.196(7) Uani 1 1 d D U . . .
H14A H 0.1137 0.2092 0.7519 0.236 Uiso 1 1 calc R U . . .
H14B H 0.0526 0.1943 0.6780 0.236 Uiso 1 1 calc R U . . .
C15 C 0.1033(15) 0.1560(12) 0.612(2) 0.324(15) Uani 1 1 d D U . . .
H15A H 0.1475 0.1727 0.5900 0.487 Uiso 1 1 calc R U . . .
H15B H 0.0770 0.1443 0.5441 0.487 Uiso 1 1 calc R U . . .
H15C H 0.0897 0.1188 0.6595 0.487 Uiso 1 1 calc R U . . .
C16 C 0.3510(7) 0.5028(8) 1.1608(11) 0.121(4) Uani 1 1 d . . . . .
C17 C 0.4598(4) 1.0000 0.2500 0.222(12) Uani 1 2 d DS TU P . .
C18 C 0.6667 0.3333 0.5741(15) 0.211(15) Uani 1 3 d DS T P . .
Cl1 Cl 0.39146(16) 1.0000 0.2500 0.1090(14) Uani 1 2 d DS T P . .
Cl2 Cl 0.4995(5) 1.0105(5) 0.1234(8) 0.231(6) Uani 0.6 1 d D U P . .
Cl3 Cl 0.6306(5) 0.2596(3) 0.6260(8) 0.329(8) Uani 0.75 1 d D U P . .
Cl3' Cl 0.6667 0.3333 0.4285(8) 0.314(10) Uani 0.75 3 d DS TU P . .
Cl2' Cl 0.4650(9) 0.9521(9) 0.3513(14) 0.272(11) Uani 0.4 1 d D U P . .


_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
S1 C12 1.760(11) 4_556 ?
S1 C2 1.801(10) . ?
S2 C8 1.761(9) . ?
S2 C6 1.798(9) . ?
O1 C1 1.360(10) . ?
O1 C13 1.446(12) . ?
O2 C7 1.312(11) . ?
N1 C16 1.133(16) . ?
C1 C2 1.383(12) . ?
C1 C6 1.395(12) . ?
C2 C3 1.366(13) . ?
C3 C4 1.369(14) . ?
C4 C5 1.369(14) . ?
C5 C6 1.402(14) . ?
C7 C8 1.428(13) . ?
C7 C12 1.451(12) . ?
C8 C9 1.396(14) . ?
C9 C10 1.411(13) . ?
C10 C11 1.356(14) . ?
C10 C16 1.421(19) . ?
C11 C12 1.345(14) . ?
C12 S1 1.760(11) 4_556 ?
C13 C14 1.62(2) . ?
C14 C15 1.447(17) . ?
C17 Cl1 1.639(8) . ?
C17 Cl2' 1.695(8) 5_675 ?
C17 Cl2' 1.695(8) . ?
C17 Cl2 1.705(5) . ?
C17 Cl2 1.705(5) 5_675 ?
C18 Cl3 1.647(9) 2_655 ?
C18 Cl3 1.647(9) . ?
C18 Cl3 1.647(9) 3_665 ?
C18 Cl3' 1.696(17) . ?
Cl2 Cl2' 0.842(19) 5_675 ?
Cl2' Cl2 0.842(19) 5_675 ?

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
C12 S1 C2 101.3(4) 4_556 . ?
C8 S2 C6 101.8(4) . . ?
C1 O1 C13 114.3(7) . . ?
O1 C1 C2 120.9(9) . . ?
O1 C1 C6 120.2(8) . . ?
C2 C1 C6 118.7(9) . . ?
C3 C2 C1 119.4(9) . . ?
C3 C2 S1 119.4(7) . . ?
C1 C2 S1 121.2(8) . . ?
C2 C3 C4 122.6(9) . . ?
C5 C4 C3 119.2(10) . . ?
C4 C5 C6 119.3(10) . . ?
C1 C6 C5 120.7(8) . . ?
C1 C6 S2 119.4(8) . . ?
C5 C6 S2 119.7(7) . . ?
O2 C7 C8 123.7(8) . . ?
O2 C7 C12 118.8(9) . . ?
C8 C7 C12 117.5(9) . . ?
C9 C8 C7 120.2(9) . . ?
C9 C8 S2 120.1(8) . . ?
C7 C8 S2 119.5(8) . . ?
C8 C9 C10 119.3(10) . . ?
C11 C10 C9 120.3(10) . . ?
C11 C10 C16 119.8(10) . . ?
C9 C10 C16 119.9(11) . . ?
C12 C11 C10 122.9(9) . . ?
C11 C12 C7 119.7(10) . . ?
C11 C12 S1 120.9(7) . 4_556 ?
C7 C12 S1 119.2(8) . 4_556 ?
O1 C13 C14 104.5(10) . . ?
C15 C14 C13 104.0(18) . . ?
N1 C16 C10 177.2(17) . . ?
Cl1 C17 Cl2' 114.4(7) . 5_675 ?
Cl1 C17 Cl2' 114.4(7) . . ?
Cl2' C17 Cl2' 131.2(13) 5_675 . ?
Cl1 C17 Cl2 119.0(6) . . ?
Cl2' C17 Cl2 28.7(6) 5_675 . ?
Cl2' C17 Cl2 118.4(7) . . ?
Cl1 C17 Cl2 119.0(6) . 5_675 ?
Cl2' C17 Cl2 118.4(7) 5_675 5_675 ?
Cl2' C17 Cl2 28.7(6) . 5_675 ?
Cl2 C17 Cl2 121.9(11) . 5_675 ?
Cl3 C18 Cl3 107.3(7) 2_655 . ?
Cl3 C18 Cl3 107.3(7) 2_655 3_665 ?
Cl3 C18 Cl3 107.3(7) . 3_665 ?
Cl3 C18 Cl3' 111.5(7) 2_655 . ?
Cl3 C18 Cl3' 111.5(6) . . ?
Cl3 C18 Cl3' 111.5(6) 3_665 . ?
Cl2' Cl2 C17 75.0(7) 5_675 . ?
Cl2 Cl2' C17 76.3(8) 5_675 . ?

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
C13 O1 C1 C2 -92.4(11) . . . . ?
C13 O1 C1 C6 93.2(11) . . . . ?
O1 C1 C2 C3 -177.2(8) . . . . ?
C6 C1 C2 C3 -2.8(12) . . . . ?
O1 C1 C2 S1 3.8(11) . . . . ?
C6 C1 C2 S1 178.3(6) . . . . ?
C12 S1 C2 C3 76.9(8) 4_556 . . . ?
C12 S1 C2 C1 -104.1(7) 4_556 . . . ?
C1 C2 C3 C4 1.7(14) . . . . ?
S1 C2 C3 C4 -179.3(8) . . . . ?
C2 C3 C4 C5 -0.8(15) . . . . ?
C3 C4 C5 C6 0.9(14) . . . . ?
O1 C1 C6 C5 177.5(7) . . . . ?
C2 C1 C6 C5 2.9(12) . . . . ?
O1 C1 C6 S2 -8.2(10) . . . . ?
C2 C1 C6 S2 177.3(6) . . . . ?
C4 C5 C6 C1 -2.0(13) . . . . ?
C4 C5 C6 S2 -176.3(7) . . . . ?
C8 S2 C6 C1 102.3(7) . . . . ?
C8 S2 C6 C5 -83.3(8) . . . . ?
O2 C7 C8 C9 -178.9(8) . . . . ?
C12 C7 C8 C9 2.4(12) . . . . ?
O2 C7 C8 S2 6.2(12) . . . . ?
C12 C7 C8 S2 -172.5(6) . . . . ?
C6 S2 C8 C9 106.0(8) . . . . ?
C6 S2 C8 C7 -79.1(8) . . . . ?
C7 C8 C9 C10 -1.3(13) . . . . ?
S2 C8 C9 C10 173.6(7) . . . . ?
C8 C9 C10 C11 -1.7(13) . . . . ?
C8 C9 C10 C16 178.0(9) . . . . ?
C9 C10 C11 C12 3.7(14) . . . . ?
C16 C10 C11 C12 -176.0(10) . . . . ?
C10 C11 C12 C7 -2.5(14) . . . . ?
C10 C11 C12 S1 -177.1(7) . . . 4_556 ?
O2 C7 C12 C11 -179.3(8) . . . . ?
C8 C7 C12 C11 -0.5(12) . . . . ?
O2 C7 C12 S1 -4.7(11) . . . 4_556 ?
C8 C7 C12 S1 174.2(7) . . . 4_556 ?
C1 O1 C13 C14 -167.0(10) . . . . ?
O1 C13 C14 C15 -86.0(19) . . . . ?
Cl1 C17 Cl2 Cl2' 88.2(19) . . . 5_675 ?
Cl2' C17 Cl2 Cl2' -125(2) . . . 5_675 ?
Cl2 C17 Cl2 Cl2' -91.8(19) 5_675 . . 5_675 ?
Cl1 C17 Cl2' Cl2 -106.4(18) . . . 5_675 ?
Cl2' C17 Cl2' Cl2 73.6(18) 5_675 . . 5_675 ?
Cl2 C17 Cl2' Cl2 105(2) . . . 5_675 ?

_refine_diff_density_max         1.199
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.115

_shelxl_version_number           2013-2


# start Validation Reply Form

_vrf_PLAT234_12.CHCl3            
;
PROBLEM: Large Hirshfeld Difference C14 -- C15 .. 0.37 Ang	
RESPONSE: This is due to the weak diffraction ability of the crystal selected
for x-ray diffraction experiment. Although several times have been tried to
select better crystals, we are failed each time.
;

#===END
