# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_keinan31
_database_code_depnum_ccdc_archive 'CCDC 1040969'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Pentakis(t-butylsulfido)corannulene
_chemical_name_common            Keinan-31
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H50 S5'
_chemical_formula_weight         691.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'

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

_cell_length_a                   20.235(4)
_cell_length_b                   6.7830(10)
_cell_length_c                   27.996(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3842.6(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22820
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      25.58

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22820
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0525
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         25.58
_reflns_number_total             3621
_reflns_number_gt                2434
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius, 2006)'
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1213P)²+6.0039P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_number_reflns         3621
_refine_ls_number_parameters     388
_refine_ls_number_restraints     57
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0791
_refine_ls_wR_factor_ref         0.2449
_refine_ls_wR_factor_gt          0.2085
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.183
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

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
S1 S 0.80880(16) -0.1058(5) 0.31478(10) 0.0463(8) Uani 1 1 d D . .
S2 S 1.00443(16) -0.6649(4) 0.37663(12) 0.0465(8) Uani 1 1 d D . .
S3 S 1.00412(17) -0.6637(5) 0.57881(11) 0.0478(8) Uani 1 1 d D . .
S4 S 0.80888(15) -0.1050(5) 0.64117(10) 0.0446(8) Uani 1 1 d D . .
S5 S 0.69633(10) 0.2522(3) 0.47764(15) 0.0450(5) Uani 1 1 d D . .
C1 C 0.8679(5) -0.1279(15) 0.3635(4) 0.091(6) Uani 1 1 d D . .
C2 C 0.9170(5) -0.2785(16) 0.3658(4) 0.0547(14) Uani 1 1 d D . .
H2 H 0.9247 -0.3588 0.3395 0.066 Uiso 1 1 calc R . .
C3 C 0.9524(5) -0.3044(16) 0.4062(4) 0.054(3) Uani 1 1 d D . .
C4 C 0.9868(6) -0.4772(13) 0.4208(3) 0.069(4) Uani 1 1 d D . .
C5 C 1.0012(5) -0.5217(17) 0.4698(3) 0.0547(14) Uani 1 1 d D . .
H5 H 1.0232 -0.6378 0.4775 0.066 Uiso 1 1 calc R . .
C6 C 0.9825(6) -0.3935(19) 0.5057(3) 0.060(3) Uani 1 1 d D . .
C7 C 0.9707(5) -0.4346(15) 0.5545(3) 0.070(4) Uani 1 1 d D . .
C8 C 0.9269(6) -0.3147(16) 0.5838(4) 0.0547(14) Uani 1 1 d D . .
H8 H 0.9173 -0.3493 0.6152 0.066 Uiso 1 1 calc R . .
C9 C 0.9000(5) -0.1470(18) 0.5632(4) 0.060(3) Uani 1 1 d D . .
C10 C 0.8445(5) -0.0541(17) 0.5834(3) 0.0547(14) Uani 1 1 d D . .
C11 C 0.8129(9) 0.0699(18) 0.5486(4) 0.166(14) Uani 1 1 d D . .
H11 H 0.7808 0.1468 0.5634 0.199 Uiso 1 1 calc R . .
C12 C 0.8147(7) 0.1120(16) 0.5004(4) 0.070(4) Uani 1 1 d D . .
C13 C 0.7763(5) 0.1532(18) 0.4590(5) 0.20(2) Uani 1 1 d D . .
C14 C 0.7990(5) 0.0947(15) 0.4122(4) 0.047(3) Uani 1 1 d D . .
H14 H 0.7722 0.1307 0.3867 0.057 Uiso 1 1 calc R . .
C15 C 0.8517(8) -0.0010(17) 0.4016(6) 0.124(9) Uani 1 1 d D . .
C16 C 0.9014(10) -0.027(3) 0.4433(6) 0.094(8) Uani 1 1 d . . .
C17 C 0.9475(9) -0.167(3) 0.4474(7) 0.094(7) Uani 1 1 d . . .
C18 C 0.9547(7) -0.202(2) 0.4931(10) 0.101(9) Uani 1 1 d . . .
C19 C 0.9138(10) -0.083(3) 0.5176(4) 0.086(7) Uani 1 1 d . . .
C20 C 0.8829(6) 0.0316(18) 0.4853(9) 0.080(6) Uani 1 1 d . . .
C21 C 0.8472(7) 0.084(2) 0.2741(4) 0.054(4) Uani 1 1 d . . .
C22 C 0.8404(9) 0.292(2) 0.2951(5) 0.071(5) Uani 1 1 d . . .
H22A H 0.7946 0.3204 0.3006 0.106 Uiso 1 1 calc R . .
H22B H 0.8584 0.3865 0.2732 0.106 Uiso 1 1 calc R . .
H22C H 0.8640 0.2988 0.3248 0.106 Uiso 1 1 calc R . .
C23 C 0.8051(9) 0.068(2) 0.2292(6) 0.072(5) Uani 1 1 d . . .
H23A H 0.7606 0.1068 0.2364 0.109 Uiso 1 1 calc R . .
H23B H 0.8055 -0.0657 0.2180 0.109 Uiso 1 1 calc R . .
H23C H 0.8227 0.1530 0.2049 0.109 Uiso 1 1 calc R . .
C24 C 0.9200(8) 0.023(3) 0.2660(6) 0.074(5) Uani 1 1 d . . .
H24A H 0.9439 0.0339 0.2955 0.111 Uiso 1 1 calc R . .
H24B H 0.9396 0.1079 0.2426 0.111 Uiso 1 1 calc R . .
H24C H 0.9215 -0.1109 0.2550 0.111 Uiso 1 1 calc R . .
C25 C 1.0743(7) -0.570(2) 0.3409(5) 0.057(4) Uani 1 1 d . . .
C26 C 1.1153(7) -0.434(3) 0.3701(6) 0.080(5) Uani 1 1 d . . .
H26A H 1.1269 -0.4977 0.3996 0.120 Uiso 1 1 calc R . .
H26B H 1.0907 -0.3164 0.3767 0.120 Uiso 1 1 calc R . .
H26C H 1.1548 -0.4013 0.3528 0.120 Uiso 1 1 calc R . .
C27 C 1.0541(10) -0.490(3) 0.2931(6) 0.093(5) Uani 1 1 d . . .
H27A H 1.0274 -0.5852 0.2767 0.139 Uiso 1 1 calc R . .
H27B H 1.0928 -0.4616 0.2744 0.139 Uiso 1 1 calc R . .
H27C H 1.0291 -0.3706 0.2975 0.139 Uiso 1 1 calc R . .
C28 C 1.1149(9) -0.757(3) 0.3304(8) 0.106(8) Uani 1 1 d . . .
H28A H 1.1330 -0.8070 0.3597 0.159 Uiso 1 1 calc R . .
H28B H 1.1502 -0.7252 0.3088 0.159 Uiso 1 1 calc R . .
H28C H 1.0868 -0.8546 0.3162 0.159 Uiso 1 1 calc R . .
C29 C 1.0753(6) -0.5759(19) 0.6157(5) 0.051(4) Uani 1 1 d . . .
C30 C 1.1174(8) -0.424(3) 0.5883(7) 0.090(6) Uani 1 1 d . . .
H30A H 1.0911 -0.3103 0.5813 0.136 Uiso 1 1 calc R . .
H30B H 1.1328 -0.4820 0.5590 0.136 Uiso 1 1 calc R . .
H30C H 1.1546 -0.3865 0.6075 0.136 Uiso 1 1 calc R . .
C31 C 1.0467(9) -0.472(4) 0.6590(6) 0.124(9) Uani 1 1 d . . .
H31A H 1.0217 -0.3591 0.6488 0.186 Uiso 1 1 calc R . .
H31B H 1.0819 -0.4299 0.6796 0.186 Uiso 1 1 calc R . .
H31C H 1.0182 -0.5608 0.6761 0.186 Uiso 1 1 calc R . .
C32 C 1.1131(11) -0.756(4) 0.6255(8) 0.130(9) Uani 1 1 d . . .
H32A H 1.0865 -0.8452 0.6439 0.195 Uiso 1 1 calc R . .
H32B H 1.1523 -0.7230 0.6432 0.195 Uiso 1 1 calc R . .
H32C H 1.1253 -0.8171 0.5959 0.195 Uiso 1 1 calc R . .
C33 C 0.8454(6) 0.0785(17) 0.6802(4) 0.038(3) Uani 1 1 d . . .
C34 C 0.8399(9) 0.2815(18) 0.6600(5) 0.070(5) Uani 1 1 d . . .
H34A H 0.8665 0.2911 0.6317 0.105 Uiso 1 1 calc R . .
H34B H 0.8552 0.3754 0.6832 0.105 Uiso 1 1 calc R . .
H34C H 0.7946 0.3086 0.6522 0.105 Uiso 1 1 calc R . .
C35 C 0.8054(8) 0.060(2) 0.7266(4) 0.067(5) Uani 1 1 d . . .
H35A H 0.8116 -0.0689 0.7400 0.101 Uiso 1 1 calc R . .
H35B H 0.7594 0.0805 0.7199 0.101 Uiso 1 1 calc R . .
H35C H 0.8203 0.1576 0.7491 0.101 Uiso 1 1 calc R . .
C36 C 0.9185(7) 0.038(3) 0.6905(6) 0.078(5) Uani 1 1 d . . .
H36A H 0.9232 -0.0907 0.7041 0.117 Uiso 1 1 calc R . .
H36B H 0.9348 0.1350 0.7126 0.117 Uiso 1 1 calc R . .
H36C H 0.9432 0.0461 0.6613 0.117 Uiso 1 1 calc R . .
C37 C 0.7085(6) 0.5211(13) 0.4761(7) 0.067(3) Uani 1 1 d . . .
C38 C 0.7371(9) 0.581(2) 0.4312(7) 0.092(6) Uani 1 1 d . . .
H38A H 0.7818 0.5347 0.4293 0.138 Uiso 1 1 calc R . .
H38B H 0.7367 0.7226 0.4290 0.138 Uiso 1 1 calc R . .
H38C H 0.7119 0.5268 0.4053 0.138 Uiso 1 1 calc R . .
C39 C 0.6380(6) 0.5973(18) 0.4798(9) 0.093(4) Uani 1 1 d . . .
H39A H 0.6170 0.5400 0.5072 0.139 Uiso 1 1 calc R . .
H39B H 0.6140 0.5618 0.4515 0.139 Uiso 1 1 calc R . .
H39C H 0.6386 0.7382 0.4830 0.139 Uiso 1 1 calc R . .
C40 C 0.7510(13) 0.583(2) 0.5207(10) 0.174(13) Uani 1 1 d . . .
H40A H 0.7286 0.5443 0.5494 0.261 Uiso 1 1 calc R . .
H40B H 0.7568 0.7239 0.5206 0.261 Uiso 1 1 calc R . .
H40C H 0.7933 0.5201 0.5192 0.261 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.821(9) . ?
S1 C21 1.888(12) . ?
S2 C4 1.810(8) . ?
S2 C25 1.849(16) . ?
S3 C7 1.825(8) . ?
S3 C29 1.871(13) . ?
S4 C10 1.804(8) . ?
S4 C33 1.812(13) . ?
S5 C13 1.827(9) . ?
S5 C37 1.841(9) . ?
C1 C15 1.408(9) . ?
C1 C2 1.426(8) . ?
C2 C3 1.350(16) . ?
C2 H2 0.9300 . ?
C3 C4 1.424(8) . ?
C3 C17 1.486(19) . ?
C4 C5 1.435(8) . ?
C5 C6 1.382(15) . ?
C5 H5 0.9300 . ?
C6 C7 1.414(8) . ?
C6 C18 1.457(18) . ?
C7 C8 1.456(8) . ?
C8 C9 1.388(14) . ?
C8 H8 0.9300 . ?
C9 C19 1.376(17) . ?
C9 C10 1.407(8) . ?
C10 C11 1.437(9) . ?
C11 C12 1.378(14) . ?
C11 H11 0.9300 . ?
C12 C13 1.424(8) . ?
C12 C20 1.543(18) . ?
C13 C14 1.445(9) . ?
C14 C15 1.283(16) . ?
C14 H14 0.9300 . ?
C15 C16 1.55(2) . ?
C16 C20 1.30(3) . ?
C16 C17 1.33(3) . ?
C17 C18 1.31(3) . ?
C18 C19 1.34(3) . ?
C19 C20 1.35(3) . ?
C21 C23 1.52(2) . ?
C21 C22 1.53(2) . ?
C21 C24 1.55(2) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.48(2) . ?
C25 C27 1.50(2) . ?
C25 C28 1.54(2) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C32 1.47(2) . ?
C29 C31 1.52(2) . ?
C29 C30 1.540(19) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.492(18) . ?
C33 C36 1.532(18) . ?
C33 C35 1.537(16) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.44(2) . ?
C37 C39 1.519(15) . ?
C37 C40 1.57(2) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C21 103.8(6) . . ?
C4 S2 C25 106.0(6) . . ?
C7 S3 C29 102.7(6) . . ?
C10 S4 C33 104.2(5) . . ?
C13 S5 C37 103.8(6) . . ?
C15 C1 C2 124.5(11) . . ?
C15 C1 S1 111.3(11) . . ?
C2 C1 S1 123.4(8) . . ?
C3 C2 C1 120.0(10) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 127.4(11) . . ?
C2 C3 C17 122.2(14) . . ?
C4 C3 C17 109.0(13) . . ?
C3 C4 C5 123.1(9) . . ?
C3 C4 S2 118.6(8) . . ?
C5 C4 S2 117.8(7) . . ?
C6 C5 C4 120.5(10) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 128.7(11) . . ?
C5 C6 C18 119.3(15) . . ?
C7 C6 C18 110.2(15) . . ?
C6 C7 C8 122.4(9) . . ?
C6 C7 S3 117.7(8) . . ?
C8 C7 S3 119.4(7) . . ?
C9 C8 C7 117.6(9) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
C19 C9 C8 124.4(14) . . ?
C19 C9 C10 113.2(13) . . ?
C8 C9 C10 120.9(11) . . ?
C9 C10 C11 110.1(10) . . ?
C9 C10 S4 126.4(9) . . ?
C11 C10 S4 122.9(7) . . ?
C12 C11 C10 140.6(15) . . ?
C12 C11 H11 109.7 . . ?
C10 C11 H11 109.7 . . ?
C11 C12 C13 145.3(15) . . ?
C11 C12 C20 102.7(16) . . ?
C13 C12 C20 109.5(12) . . ?
C12 C13 C14 120.8(8) . . ?
C12 C13 S5 108.9(10) . . ?
C14 C13 S5 129.9(9) . . ?
C15 C14 C13 127.8(12) . . ?
C15 C14 H14 116.1 . . ?
C13 C14 H14 116.1 . . ?
C14 C15 C1 132.7(17) . . ?
C14 C15 C16 115.0(16) . . ?
C1 C15 C16 110.3(13) . . ?
C20 C16 C17 110.1(14) . . ?
C20 C16 C15 117(2) . . ?
C17 C16 C15 126.9(19) . . ?
C18 C17 C16 106.9(15) . . ?
C18 C17 C3 130(2) . . ?
C16 C17 C3 115.1(19) . . ?
C17 C18 C19 108.6(15) . . ?
C17 C18 C6 116(2) . . ?
C19 C18 C6 131(2) . . ?
C20 C19 C18 106.9(15) . . ?
C20 C19 C9 135(2) . . ?
C18 C19 C9 114(2) . . ?
C16 C20 C19 107.2(14) . . ?
C16 C20 C12 128.1(19) . . ?
C19 C20 C12 115.7(18) . . ?
C23 C21 C22 109.5(12) . . ?
C23 C21 C24 113.1(12) . . ?
C22 C21 C24 112.9(12) . . ?
C23 C21 S1 102.6(9) . . ?
C22 C21 S1 111.0(9) . . ?
C24 C21 S1 107.2(10) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C27 114.8(15) . . ?
C26 C25 C28 108.5(13) . . ?
C27 C25 C28 105.9(15) . . ?
C26 C25 S2 110.2(9) . . ?
C27 C25 S2 113.6(11) . . ?
C28 C25 S2 102.9(11) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C32 C29 C31 115.9(17) . . ?
C32 C29 C30 111.1(15) . . ?
C31 C29 C30 107.4(16) . . ?
C32 C29 S3 103.9(12) . . ?
C31 C29 S3 107.1(10) . . ?
C30 C29 S3 111.3(10) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C36 107.8(13) . . ?
C34 C33 C35 110.8(10) . . ?
C36 C33 C35 109.5(11) . . ?
C34 C33 S4 112.1(9) . . ?
C36 C33 S4 112.7(9) . . ?
C35 C33 S4 103.9(9) . . ?
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 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C39 109.9(14) . . ?
C38 C37 C40 113.3(13) . . ?
C39 C37 C40 111.5(17) . . ?
C38 C37 S5 110.8(12) . . ?
C39 C37 S5 102.1(8) . . ?
C40 C37 S5 108.7(10) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
# start Validation Reply Form
_vrf_PLAT213_keinan31
;
PROBLEM: Atom C11 has ADP max/min Ratio ...22.50 prola
RESPONSE: At Part of the carbon atoms there are unresolved disorder.
Refinement was done with restrains   
;
_vrf_PLAT220_keinan31            
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ..5.53 Ratio
RESPONSE: At Part of the carbon atoms there are unresolved disorder.
Refinement was done with restrains
;
_vrf_PLAT241_keinan31            
;
PROBLEM: Check High Ueq as Compared to Neighbors for  C11     
RESPONSE: At Part of the carbon atoms there are unresolved disorder.
Refinement was done with restrains
;
_vrf_PLAT242_keinan31            
;
PROBLEM: Check Low  Ueq as Compared to Neighbors for S5     
RESPONSE: Neighbors carbon atoms are disordered
;
# end Validation Reply Form

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        25.58
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.089
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane'
####################################################################### 
# 
# 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_Keinan-43
_database_code_depnum_ccdc_archive 'CCDC 1040970'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Decakis(t-butylsulfido)corannulene
_chemical_name_common            'Keinan-43 polymorph B'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H90 S10'
_chemical_formula_weight         1131.92

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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P n'

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

_cell_length_a                   10.370(2)
_cell_length_b                   21.376(4)
_cell_length_c                   14.870(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.74(2)
_cell_angle_gamma                90.00
_cell_volume                     3295.9(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    23464
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      25.10

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1220
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23464
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_sigmaI/netI    0.1175
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         25.02
_reflns_number_total             5555
_reflns_number_gt                1773
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius, 2006)'
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1729P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5555
_refine_ls_number_parameters     565
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.2521
_refine_ls_R_factor_gt           0.0968
_refine_ls_wR_factor_ref         0.3063
_refine_ls_wR_factor_gt          0.2413
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_restrained_S_all      0.874
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.012

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
S1 S 0.9682(6) 0.3765(3) 0.7081(4) 0.124(2) Uani 1 1 d D . .
S4 S 0.6328(6) 0.0427(2) 0.5598(4) 0.1096(19) Uani 1 1 d . . .
S2 S 0.8971(6) 0.2408(3) 0.7812(4) 0.123(2) Uani 1 1 d D . .
S8 S 0.8843(7) 0.3745(3) 0.1631(4) 0.123(2) Uani 1 1 d . . .
S5 S 0.4988(6) 0.0718(2) 0.3685(5) 0.126(2) Uani 1 1 d . . .
S9 S 0.9655(7) 0.4577(2) 0.3312(5) 0.121(2) Uani 1 1 d . . .
S6 S 0.6312(6) 0.1219(3) 0.1850(4) 0.1157(19) Uani 1 1 d . . .
S3 S 0.7165(7) 0.1271(3) 0.7319(4) 0.133(2) Uani 1 1 d . . .
S7 S 0.6940(5) 0.2596(3) 0.1135(4) 0.1140(19) Uani 1 1 d D . .
S10 S 1.1009(6) 0.4286(2) 0.5274(4) 0.126(2) Uani 1 1 d . . .
C1 C 0.9551(6) 0.3329(2) 0.6013(4) 0.180(5) Uani 1 1 d R . .
C2 C 0.8697(6) 0.2828(2) 0.6026(4) 0.180(5) Uani 1 1 d RD . .
C3 C 0.7981(6) 0.2678(2) 0.5260(4) 0.180(5) Uani 1 1 d R . .
C4 C 0.8120(6) 0.3029(2) 0.4480(4) 0.180(5) Uani 1 1 d R . .
C5 C 0.8974(6) 0.3530(2) 0.4467(4) 0.180(5) Uani 1 1 d R . .
C6 C 0.9690(6) 0.3680(2) 0.5234(4) 0.180(5) Uani 1 1 d R . .
C7 C 0.8395(16) 0.2287(7) 0.6611(10) 0.154(11) Uani 1 1 d D . .
C8 C 0.762(2) 0.1696(10) 0.6458(11) 0.126(8) Uani 1 1 d D . .
C9 C 0.708(3) 0.1628(14) 0.5559(13) 0.196(14) Uani 1 1 d D . .
C10 C 0.708(2) 0.2284(10) 0.502(3) 0.26(2) Uani 1 1 d . . .
C11 C 0.654(3) 0.1095(12) 0.5086(13) 0.186(14) Uani 1 1 d D . .
C12 C 0.6120(8) 0.1250(4) 0.4159(7) 0.149(9) Uani 1 1 d D . .
C13 C 0.6597(8) 0.1741(4) 0.3594(7) 0.211(14) Uani 1 1 d R . .
C15 C 0.6757(8) 0.1796(4) 0.2670(7) 0.100(5) Uani 1 1 d R . .
C16 C 0.7275(8) 0.2341(4) 0.2313(7) 0.121(7) Uani 1 1 d R . .
C17 C 0.7633(8) 0.2830(4) 0.2879(7) 0.228(18) Uani 1 1 d RD . .
C18 C 0.7473(8) 0.2775(4) 0.3802(7) 0.164(10) Uani 1 1 d R . .
C14 C 0.6955(8) 0.2231(4) 0.4159(7) 0.44(5) Uani 1 1 d R . .
C19 C 0.8616(19) 0.3384(8) 0.2822(15) 0.140(9) Uani 1 1 d D . .
C20 C 0.924(2) 0.3818(7) 0.3576(14) 0.121(8) Uani 1 1 d D . .
C21 C 0.8229(18) 0.4201(12) 0.7302(13) 0.134(9) Uani 1 1 d D . .
C22 C 0.706(2) 0.4058(19) 0.6685(19) 0.227(17) Uani 1 1 d . . .
H22A H 0.7020 0.3616 0.6572 0.341 Uiso 1 1 calc R . .
H22B H 0.7153 0.4277 0.6126 0.341 Uiso 1 1 calc R . .
H22C H 0.6285 0.4191 0.6973 0.341 Uiso 1 1 calc R . .
C23 C 0.779(4) 0.404(3) 0.817(3) 0.36(4) Uani 1 1 d . . .
H23A H 0.7579 0.3600 0.8180 0.538 Uiso 1 1 calc R . .
H23B H 0.7039 0.4279 0.8308 0.538 Uiso 1 1 calc R . .
H23C H 0.8458 0.4121 0.8606 0.538 Uiso 1 1 calc R . .
C24 C 0.850(4) 0.4888(10) 0.715(3) 0.30(3) Uani 1 1 d . . .
H24A H 0.9214 0.5015 0.7528 0.454 Uiso 1 1 calc R . .
H24B H 0.7750 0.5128 0.7308 0.454 Uiso 1 1 calc R . .
H24C H 0.8702 0.4957 0.6535 0.454 Uiso 1 1 calc R . .
C25 C 1.0488(16) 0.1982(13) 0.7798(15) 0.23(2) Uani 1 1 d D . .
C26 C 1.089(3) 0.1717(12) 0.694(2) 0.218(15) Uani 1 1 d D . .
H26A H 1.1206 0.2045 0.6556 0.326 Uiso 1 1 calc R . .
H26B H 1.0171 0.1515 0.6647 0.326 Uiso 1 1 calc R . .
H26C H 1.1566 0.1416 0.7040 0.326 Uiso 1 1 calc R . .
C27 C 1.010(5) 0.149(2) 0.841(3) 0.85(14) Uani 1 1 d D . .
H27A H 0.9326 0.1292 0.8192 1.275 Uiso 1 1 calc R . .
H27B H 0.9950 0.1661 0.8998 1.275 Uiso 1 1 calc R . .
H27C H 1.0775 0.1179 0.8458 1.275 Uiso 1 1 calc R . .
C28 C 1.152(3) 0.237(2) 0.819(2) 0.41(4) Uani 1 1 d D . .
H28A H 1.1354 0.2800 0.8076 0.617 Uiso 1 1 calc R . .
H28B H 1.2333 0.2251 0.7934 0.617 Uiso 1 1 calc R . .
H28C H 1.1564 0.2298 0.8833 0.617 Uiso 1 1 calc R . .
C29 C 0.572(3) 0.1565(15) 0.7750(16) 0.209(16) Uani 1 1 d D . .
C30 C 0.467(3) 0.130(3) 0.720(2) 0.44(5) Uani 1 1 d D . .
H30A H 0.4652 0.1500 0.6622 0.661 Uiso 1 1 calc R . .
H30B H 0.3864 0.1367 0.7495 0.661 Uiso 1 1 calc R . .
H30C H 0.4810 0.0859 0.7126 0.661 Uiso 1 1 calc R . .
C31 C 0.557(6) 0.1358(15) 0.869(2) 0.41(5) Uani 1 1 d D . .
H31A H 0.5356 0.0921 0.8696 0.612 Uiso 1 1 calc R . .
H31B H 0.4893 0.1594 0.8962 0.612 Uiso 1 1 calc R . .
H31C H 0.6363 0.1425 0.9013 0.612 Uiso 1 1 calc R . .
C32 C 0.567(3) 0.2247(17) 0.772(3) 0.34(4) Uani 1 1 d D . .
H32A H 0.6210 0.2395 0.7243 0.513 Uiso 1 1 calc R . .
H32B H 0.5960 0.2416 0.8280 0.513 Uiso 1 1 calc R . .
H32C H 0.4795 0.2378 0.7600 0.513 Uiso 1 1 calc R . .
C33 C 0.773(3) -0.0060(10) 0.5381(19) 0.137(9) Uani 1 1 d . . .
C34 C 0.880(3) 0.025(3) 0.576(6) 0.54(8) Uani 1 1 d . . .
H34A H 0.8778 0.0682 0.5593 0.805 Uiso 1 1 calc R . .
H34B H 0.9575 0.0060 0.5551 0.805 Uiso 1 1 calc R . .
H34C H 0.8767 0.0215 0.6406 0.805 Uiso 1 1 calc R . .
C35 C 0.756(4) -0.0666(14) 0.568(2) 0.243(19) Uani 1 1 d . . .
H35A H 0.7481 -0.0666 0.6322 0.364 Uiso 1 1 calc R . .
H35B H 0.8283 -0.0915 0.5511 0.364 Uiso 1 1 calc R . .
H35C H 0.6785 -0.0837 0.5413 0.364 Uiso 1 1 calc R . .
C36 C 0.766(3) -0.0182(12) 0.4308(18) 0.217(15) Uani 1 1 d . . .
H36A H 0.7745 0.0209 0.3996 0.325 Uiso 1 1 calc R . .
H36B H 0.6840 -0.0367 0.4152 0.325 Uiso 1 1 calc R . .
H36C H 0.8339 -0.0459 0.4139 0.325 Uiso 1 1 calc R . .
C37 C 0.337(2) 0.1146(12) 0.396(2) 0.135(8) Uani 1 1 d . . .
C38 C 0.317(3) 0.1643(14) 0.324(3) 0.27(2) Uani 1 1 d D . .
H38A H 0.3355 0.1468 0.2661 0.412 Uiso 1 1 calc R . .
H38B H 0.3734 0.1990 0.3357 0.412 Uiso 1 1 calc R . .
H38C H 0.2289 0.1785 0.3245 0.412 Uiso 1 1 calc R . .
C39 C 0.313(4) 0.133(2) 0.483(2) 0.35(4) Uani 1 1 d D . .
H39A H 0.3403 0.1008 0.5240 0.527 Uiso 1 1 calc R . .
H39B H 0.2228 0.1409 0.4901 0.527 Uiso 1 1 calc R . .
H39C H 0.3607 0.1707 0.4960 0.527 Uiso 1 1 calc R . .
C40 C 0.247(4) 0.0587(17) 0.3654(18) 0.249(18) Uani 1 1 d D . .
H40A H 0.2688 0.0467 0.3053 0.374 Uiso 1 1 calc R . .
H40B H 0.1588 0.0716 0.3671 0.374 Uiso 1 1 calc R . .
H40C H 0.2604 0.0238 0.4052 0.374 Uiso 1 1 calc R . .
C41 C 0.788(3) 0.0812(11) 0.1537(18) 0.24(2) Uani 1 1 d D . .
C42 C 0.789(5) 0.089(2) 0.0535(19) 0.44(5) Uani 1 1 d D . .
H42A H 0.7108 0.0722 0.0280 0.655 Uiso 1 1 calc R . .
H42B H 0.8617 0.0681 0.0290 0.655 Uiso 1 1 calc R . .
H42C H 0.7937 0.1331 0.0393 0.655 Uiso 1 1 calc R . .
C43 C 0.905(3) 0.1087(17) 0.197(3) 0.38(4) Uani 1 1 d D . .
H43A H 0.8911 0.1136 0.2606 0.570 Uiso 1 1 calc R . .
H43B H 0.9230 0.1488 0.1711 0.570 Uiso 1 1 calc R . .
H43C H 0.9777 0.0814 0.1884 0.570 Uiso 1 1 calc R . .
C44 C 0.762(4) 0.0160(15) 0.181(3) 0.47(5) Uani 1 1 d D . .
H44A H 0.7662 0.0129 0.2453 0.702 Uiso 1 1 calc R . .
H44B H 0.8257 -0.0111 0.1553 0.702 Uiso 1 1 calc R . .
H44C H 0.6779 0.0039 0.1599 0.702 Uiso 1 1 calc R . .
C45 C 0.5421(17) 0.3017(9) 0.0999(16) 0.169(11) Uani 1 1 d D . .
C46 C 0.443(2) 0.2491(14) 0.120(3) 0.36(4) Uani 1 1 d D . .
H46A H 0.4462 0.2181 0.0736 0.535 Uiso 1 1 calc R . .
H46B H 0.3583 0.2666 0.1226 0.535 Uiso 1 1 calc R . .
H46C H 0.4646 0.2300 0.1770 0.535 Uiso 1 1 calc R . .
C47 C 0.539(4) 0.3558(18) 0.164(3) 0.50(7) Uani 1 1 d D . .
H47A H 0.5491 0.3407 0.2246 0.757 Uiso 1 1 calc R . .
H47B H 0.4588 0.3775 0.1579 0.757 Uiso 1 1 calc R . .
H47C H 0.6089 0.3840 0.1510 0.757 Uiso 1 1 calc R . .
C48 C 0.546(4) 0.3182(15) 0.0006(18) 0.28(2) Uani 1 1 d D . .
H48A H 0.5785 0.2831 -0.0326 0.418 Uiso 1 1 calc R . .
H48B H 0.6023 0.3535 -0.0077 0.418 Uiso 1 1 calc R . .
H48C H 0.4612 0.3285 -0.0206 0.418 Uiso 1 1 calc R . .
C49 C 1.032(2) 0.3425(11) 0.1259(14) 0.134(9) Uani 1 1 d D . .
C50 C 1.059(2) 0.2778(14) 0.146(3) 0.32(3) Uani 1 1 d D . .
H50A H 1.0579 0.2717 0.2103 0.480 Uiso 1 1 calc R . .
H50B H 1.1425 0.2670 0.1240 0.480 Uiso 1 1 calc R . .
H50C H 0.9948 0.2517 0.1183 0.480 Uiso 1 1 calc R . .
C51 C 1.025(3) 0.349(2) 0.0283(19) 0.30(3) Uani 1 1 d D . .
H51A H 1.0065 0.3918 0.0130 0.452 Uiso 1 1 calc R . .
H51B H 0.9585 0.3225 0.0045 0.452 Uiso 1 1 calc R . .
H51C H 1.1065 0.3373 0.0031 0.452 Uiso 1 1 calc R . .
C52 C 1.142(3) 0.380(2) 0.157(3) 0.43(4) Uani 1 1 d D . .
H52A H 1.1257 0.4234 0.1436 0.649 Uiso 1 1 calc R . .
H52B H 1.2180 0.3667 0.1265 0.649 Uiso 1 1 calc R . .
H52C H 1.1534 0.3748 0.2205 0.649 Uiso 1 1 calc R . .
C53 C 0.818(3) 0.5009(14) 0.357(2) 0.153(10) Uani 1 1 d . . .
C54 C 0.700(4) 0.4929(16) 0.285(3) 0.27(2) Uani 1 1 d . . .
H54A H 0.7271 0.5072 0.2269 0.400 Uiso 1 1 calc R . .
H54B H 0.6275 0.5172 0.3041 0.400 Uiso 1 1 calc R . .
H54C H 0.6759 0.4496 0.2812 0.400 Uiso 1 1 calc R . .
C55 C 0.859(5) 0.5721(12) 0.334(4) 0.37(4) Uani 1 1 d . . .
H55A H 0.9219 0.5860 0.3777 0.561 Uiso 1 1 calc R . .
H55B H 0.7840 0.5986 0.3371 0.561 Uiso 1 1 calc R . .
H55C H 0.8943 0.5740 0.2752 0.561 Uiso 1 1 calc R . .
C56 C 0.731(4) 0.479(2) 0.424(3) 0.39(4) Uani 1 1 d . . .
H56A H 0.7752 0.4777 0.4812 0.580 Uiso 1 1 calc R . .
H56B H 0.7012 0.4379 0.4085 0.580 Uiso 1 1 calc R . .
H56C H 0.6588 0.5070 0.4276 0.580 Uiso 1 1 calc R . .
C57 C 1.242(2) 0.3874(11) 0.5154(13) 0.146(9) Uani 1 1 d D . .
C58 C 1.3590(18) 0.4364(13) 0.525(2) 0.241(19) Uani 1 1 d D . .
H58A H 1.3655 0.4504 0.5865 0.361 Uiso 1 1 calc R . .
H58B H 1.3433 0.4716 0.4866 0.361 Uiso 1 1 calc R . .
H58C H 1.4381 0.4164 0.5087 0.361 Uiso 1 1 calc R . .
C59 C 1.260(3) 0.3338(14) 0.5883(16) 0.202(14) Uani 1 1 d D . .
H59A H 1.2054 0.2989 0.5727 0.303 Uiso 1 1 calc R . .
H59B H 1.2359 0.3494 0.6463 0.303 Uiso 1 1 calc R . .
H59C H 1.3480 0.3206 0.5900 0.303 Uiso 1 1 calc R . .
C60 C 1.247(3) 0.3568(12) 0.4174(19) 0.27(2) Uani 1 1 d D . .
H60A H 1.1847 0.3238 0.4129 0.400 Uiso 1 1 calc R . .
H60B H 1.3318 0.3401 0.4076 0.400 Uiso 1 1 calc R . .
H60C H 1.2283 0.3881 0.3730 0.400 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C21 1.807(15) . ?
S1 C1 1.8449 . ?
S4 C11 1.64(3) . ?
S4 C33 1.82(2) . ?
S2 C25 1.817(17) . ?
S2 C7 1.894(16) . ?
S8 C49 1.77(3) . ?
S8 C19 1.95(2) . ?
S5 C12 1.774(10) . ?
S5 C37 1.96(2) . ?
S9 C20 1.726(15) . ?
S9 C53 1.83(3) . ?
S6 C15 1.791 . ?
S6 C41 1.91(2) . ?
S3 C8 1.645(17) . ?
S3 C29 1.75(3) . ?
S7 C45 1.823(16) . ?
S7 C16 1.8629 . ?
S10 C57 1.72(3) . ?
S10 C6 1.8837 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 C3 1.3900 . ?
C2 C7 1.4830 . ?
C3 C10 1.3042 . ?
C3 C4 1.3900 . ?
C4 C18 1.3206 . ?
C4 C5 1.3900 . ?
C5 C6 1.3900 . ?
C5 C20 1.4899 . ?
C7 C8 1.512(15) . ?
C8 C9 1.449(15) . ?
C9 C11 1.45(4) . ?
C9 C10 1.62(4) . ?
C10 C14 1.2902 . ?
C11 C12 1.478(16) . ?
C12 C13 1.4374 . ?
C13 C15 1.3900 . ?
C13 C14 1.3900 . ?
C15 C16 1.3900 . ?
C16 C17 1.3900 . ?
C17 C19 1.5656 . ?
C17 C18 1.3900 . ?
C18 C14 1.3900 . ?
C19 C20 1.587(18) . ?
C21 C23 1.42(4) . ?
C21 C24 1.51(3) . ?
C21 C22 1.54(3) . ?
C25 C27 1.45(5) . ?
C25 C26 1.47(2) . ?
C25 C28 1.47(2) . ?
C29 C32 1.46(5) . ?
C29 C30 1.47(5) . ?
C29 C31 1.47(2) . ?
C33 C34 1.40(5) . ?
C33 C35 1.38(3) . ?
C33 C36 1.62(4) . ?
C37 C39 1.38(4) . ?
C37 C38 1.52(4) . ?
C37 C40 1.57(4) . ?
C41 C43 1.49(5) . ?
C41 C44 1.48(3) . ?
C41 C42 1.50(2) . ?
C45 C47 1.50(5) . ?
C45 C48 1.52(2) . ?
C45 C46 1.55(2) . ?
C49 C50 1.44(2) . ?
C49 C51 1.46(2) . ?
C49 C52 1.46(2) . ?
C53 C56 1.43(3) . ?
C53 C55 1.62(4) . ?
C53 C54 1.62(4) . ?
C57 C59 1.59(2) . ?
C57 C60 1.60(2) . ?
C57 C58 1.61(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 S1 C1 111.41 . . ?
C11 S4 C33 107.7(14) . . ?
C25 S2 C7 100.6(9) . . ?
C49 S8 C19 104.2(10) . . ?
C12 S5 C37 100.5(9) . . ?
C20 S9 C53 102.4(12) . . ?
C15 S6 C41 105.51 . . ?
C8 S3 C29 110.0(13) . . ?
C45 S7 C16 113.52 . . ?
C57 S10 C6 105.25 . . ?
C2 C1 C6 120.0 . . ?
C2 C1 S1 114.65 . . ?
C6 C1 S1 115.96 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 C7 100.74 . . ?
C1 C2 C7 138.45 . . ?
C10 C3 C2 138.32 . . ?
C10 C3 C4 101.64 . . ?
C2 C3 C4 120.0 . . ?
C18 C4 C3 110.97 . . ?
C18 C4 C5 128.59 . . ?
C3 C4 C5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C20 122.08 . . ?
C4 C5 C20 117.13 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 S10 124.4 . . ?
C1 C6 S10 115.3 . . ?
C2 C7 C8 132.75 . . ?
C2 C7 S2 112.35 . . ?
C8 C7 S2 114.6(9) . . ?
C9 C8 C7 114.9(16) . . ?
C9 C8 S3 123.4(15) . . ?
C7 C8 S3 120.1(12) . . ?
C8 C9 C11 132(3) . . ?
C8 C9 C10 112(2) . . ?
C11 C9 C10 116(2) . . ?
C14 C10 C3 113.0 . . ?
C14 C10 C9 114.55 . . ?
C3 C10 C9 115.43 . . ?
C9 C11 C12 113(2) . . ?
C9 C11 S4 120.9(17) . . ?
C12 C11 S4 126.1(17) . . ?
C13 C12 C11 127.58 . . ?
C13 C12 S5 117.85 . . ?
C11 C12 S5 114.4(13) . . ?
C15 C13 C14 120.0 . . ?
C15 C13 C12 133.3 . . ?
C14 C13 C12 106.7 . . ?
C13 C15 C16 120.0 . . ?
C13 C15 S6 125.55 . . ?
C16 C15 S6 114.48 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 S7 122.39 . . ?
C17 C16 S7 113.24 . . ?
C19 C17 C18 101.75 . . ?
C19 C17 C16 134.85 . . ?
C18 C17 C16 120.0 . . ?
C4 C18 C17 130.79 . . ?
C4 C18 C14 104.33 . . ?
C17 C18 C14 120.0 . . ?
C10 C14 C18 105.74 . . ?
C10 C14 C13 133.51 . . ?
C18 C14 C13 120.0 . . ?
C17 C19 C20 131.60 . . ?
C17 C19 S8 115.79 . . ?
C20 C19 S8 111.0(11) . . ?
C5 C20 S9 129.83 . . ?
C5 C20 C19 107.95 . . ?
S9 C20 C19 119.2(15) . . ?
C23 C21 C24 116(3) . . ?
C23 C21 C22 104(3) . . ?
C24 C21 C22 105(2) . . ?
C23 C21 S1 108.4(18) . . ?
C24 C21 S1 109(2) . . ?
C22 C21 S1 116.1(17) . . ?
C27 C25 C26 110.5(17) . . ?
C27 C25 C28 111.0(16) . . ?
C26 C25 C28 110.5(14) . . ?
C27 C25 S2 96(3) . . ?
C26 C25 S2 117.5(16) . . ?
C28 C25 S2 110(2) . . ?
C32 C29 C30 109.8(19) . . ?
C32 C29 C31 109.2(18) . . ?
C30 C29 C31 108.9(19) . . ?
C32 C29 S3 112(2) . . ?
C30 C29 S3 106.8(19) . . ?
C31 C29 S3 110(3) . . ?
C34 C33 C35 114(4) . . ?
C34 C33 C36 120(4) . . ?
C35 C33 C36 99(2) . . ?
C34 C33 S4 107(2) . . ?
C35 C33 S4 112(2) . . ?
C36 C33 S4 104.0(18) . . ?
C39 C37 C38 116(2) . . ?
C39 C37 C40 113(2) . . ?
C38 C37 C40 105(2) . . ?
C39 C37 S5 119(3) . . ?
C38 C37 S5 107(2) . . ?
C40 C37 S5 95(2) . . ?
C43 C41 C44 113.8(15) . . ?
C43 C41 C42 111.9(16) . . ?
C44 C41 C42 112.7(15) . . ?
C43 C41 S6 114(2) . . ?
C44 C41 S6 101.7(15) . . ?
C42 C41 S6 102(2) . . ?
C47 C45 C48 116.1(13) . . ?
C47 C45 C46 115(3) . . ?
C48 C45 C46 112.6(13) . . ?
C47 C45 S7 109(2) . . ?
C48 C45 S7 100.8(16) . . ?
C46 C45 S7 101.0(13) . . ?
C50 C49 C51 107.9(18) . . ?
C50 C49 C52 108.1(17) . . ?
C51 C49 C52 106.6(16) . . ?
C50 C49 S8 118.2(15) . . ?
C51 C49 S8 104.2(18) . . ?
C52 C49 S8 111(2) . . ?
C56 C53 C55 128(3) . . ?
C56 C53 C54 87(3) . . ?
C55 C53 C54 99(3) . . ?
C56 C53 S9 121(2) . . ?
C55 C53 S9 102(2) . . ?
C54 C53 S9 115.7(19) . . ?
C59 C57 C60 108.8(15) . . ?
C59 C57 C58 109.0(15) . . ?
C60 C57 C58 108.3(14) . . ?
C59 C57 S10 113.0(17) . . ?
C60 C57 S10 110.2(15) . . ?
C58 C57 S10 107.4(16) . . ?

loop_
# start Validation Reply Form
_vrf_PLAT213_Keinan-43
;
PROBLEM: Atom C14  has ADP max/min Ratio ..12.50 prola
RESPONSE: Unresolve disorder at  atom C14
;
_vrf_PLAT220_Keinan-43           
;
PROBLEM: Large Non-Solvent C  Ueq(max)/Ueq(min) ... 8.48 Ratio
RESPONSE: Most of the methyl groups are disordered
;
_vrf_PLAT241_Keinan-43           
;
PROBLEM: Check High Ueq as Compared to Neighbors for   C14     
RESPONSE: Unresolve disorder at  atom C14
;
_vrf_PLAT242_Keinan-43           
;
PROBLEM: Check Low  Ueq as Compared to Neighbors for  S2     
RESPONSE: S2 connected to disordered methyl groups
;
_vrf_PLAT224_Keinan-43           
;
PROBLEM: Ueq(Rep) and Ueq(Calc) differ by  0.006 Ang**2 .        C22      
RESPONSE: Disorder at the methyl groups lead to unusual large Uij
values
;
# end Validation Reply Form


_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.066
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Dichloromethane'
####################################################################### 
# 
# 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_Keinan-58
_database_code_depnum_ccdc_archive 'CCDC 1040971'
_audit_update_record             
;
2015-10-15 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Decakis(t-butylsulfido)corannulene
_chemical_name_common            'Keinan-58 Polymorph A'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H94.33 O2.33 S10'
_chemical_formula_weight         1173.62

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           Trigonal
_symmetry_space_group_name_H-M   'P 3'

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

_cell_length_a                   20.793(4)
_cell_length_b                   20.793(4)
_cell_length_c                   16.882(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6321(2)
_cell_formula_units_Z            3
_cell_measurement_temperature    240(1)
_cell_measurement_reflns_used    32950
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      24.73

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1899
_exptl_absorpt_coefficient_mu    0.292
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      240(1)
_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  'Nonius KappaCCD'
_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            32950
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         24.73
_reflns_number_total             7198
_reflns_number_gt                3595
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius, 2006)'
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)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     SHELXL
_refine_ls_extinction_coef       0.00290(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(2)
_refine_ls_number_reflns         7192
_refine_ls_number_parameters     611
_refine_ls_number_restraints     89
_refine_ls_R_factor_all          0.1836
_refine_ls_R_factor_gt           0.0995
_refine_ls_wR_factor_ref         0.2722
_refine_ls_wR_factor_gt          0.2371
_refine_ls_goodness_of_fit_ref   1.427
_refine_ls_restrained_S_all      1.437
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002

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
S1 S 0.388102(16) 0.135032(18) 0.60462(2) 0.08582(14) Uani 1 1 d D . .
S2 S 0.443385(16) 0.045415(17) 0.71565(2) 0.08309(13) Uani 1 1 d D . .
S3 S 0.507251(13) 0.060640(14) 0.89249(2) 0.06854(12) Uani 1 1 d D . .
S4 S 0.443262(16) 0.045684(16) 1.06969(2) 0.08222(13) Uani 1 1 d D . .
S5 S 0.388206(17) 0.133800(19) 1.18031(2) 0.08244(14) Uani 1 1 d D . .
S6 S 0.277721(17) 0.200032(19) 1.18106(2) 0.07963(14) Uani 1 1 d D . .
S7 S 0.224211(16) 0.287370(16) 1.06855(2) 0.08224(13) Uani 1 1 d D . .
S8 S 0.158891(14) 0.273612(14) 0.89259(2) 0.06905(12) Uani 1 1 d D . .
S9 S 0.224130(16) 0.287494(17) 0.71625(2) 0.08122(13) Uani 1 1 d D . .
S10 S 0.277775(17) 0.198992(19) 0.60356(2) 0.08322(14) Uani 1 1 d D . .
C1 C 0.37323(4) 0.13358(4) 0.71219(4) 0.0903(6) Uani 1 1 d D . .
C2 C 0.33467(3) 0.16383(4) 0.74149(6) 0.0733(5) Uani 1 1 d D . .
C3 C 0.33725(3) 0.16294(4) 0.82365(6) 0.0669(2) Uani 1 1 d D . .
C4 C 0.36784(4) 0.13838(5) 0.87969(4) 0.0669(2) Uani 1 1 d D . .
C5 C 0.40887(6) 0.10423(6) 0.84944(4) 0.1196(7) Uani 1 1 d D . .
C6 C 0.40672(4) 0.09749(4) 0.76528(4) 0.0780(5) Uani 1 1 d D . .
C7 C 0.43665(4) 0.08682(4) 0.91108(5) 0.1154(6) Uani 1 1 d D . .
C8 C 0.41601(4) 0.09108(3) 0.99742(5) 0.0809(5) Uani 1 1 d D . .
C9 C 0.37792(4) 0.12984(4) 1.01756(6) 0.1071(7) Uani 1 1 d D . .
C10 C 0.35060(4) 0.15245(4) 0.95340(5) 0.0669(2) Uani 1 1 d D . .
C11 C 0.35639(4) 0.14855(4) 1.08415(4) 0.0880(6) Uani 1 1 d D . .
C12 C 0.30772(4) 0.18382(4) 1.08606(4) 0.0951(7) Uani 1 1 d D . .
C13 C 0.28594(4) 0.20584(4) 1.01550(5) 0.0795(6) Uani 1 1 d D . .
C14 C 0.30939(4) 0.18658(4) 0.94488(5) 0.0669(2) Uani 1 1 d D . .
C15 C 0.30225(4) 0.19382(4) 0.86498(4) 0.0669(2) Uani 1 1 d D . .
C16 C 0.24909(4) 0.24009(4) 0.99291(5) 0.1389(8) Uani 1 1 d D . .
C17 C 0.22953(3) 0.24783(4) 0.90751(5) 0.1508(10) Uani 1 1 d D . .
C18 C 0.26157(5) 0.23053(5) 0.84123(4) 0.1083(7) Uani 1 1 d D . .
C19 C 0.26142(4) 0.23324(4) 0.76229(4) 0.1055(7) Uani 1 1 d D . .
C20 C 0.29327(4) 0.19571(4) 0.71003(5) 0.0990(7) Uani 1 1 d D . .
C21 C 0.59410(6) 0.15050(6) 0.89427(9) 0.0781(5) Uani 1 1 d . . .
C22 C 0.60916(11) 0.19231(12) 0.81205(11) 0.1904(13) Uani 1 1 d . . .
H22A H 0.5738 0.2087 0.8046 0.286 Uiso 1 1 calc R . .
H22B H 0.6043 0.1591 0.7700 0.286 Uiso 1 1 calc R . .
H22C H 0.6585 0.2345 0.8118 0.286 Uiso 1 1 calc R . .
C23 C 0.60468(11) 0.19611(14) 0.96454(15) 0.2411(15) Uani 1 1 d . . .
H23A H 0.5657 0.2080 0.9673 0.362 Uiso 1 1 calc R . .
H23B H 0.6518 0.2411 0.9612 0.362 Uiso 1 1 calc R . .
H23C H 0.6035 0.1691 1.0112 0.362 Uiso 1 1 calc R . .
C24 C 0.65543(6) 0.13611(7) 0.88372(16) 0.1868(11) Uani 1 1 d . . .
H24A H 0.6572 0.1079 0.9279 0.280 Uiso 1 1 calc R . .
H24B H 0.7013 0.1824 0.8806 0.280 Uiso 1 1 calc R . .
H24C H 0.6482 0.1085 0.8357 0.280 Uiso 1 1 calc R . .
C25 C 0.35996(3) -0.04810(4) 1.07854(4) 0.1098(6) Uani 1 1 d D . .
C26 C 0.38415(6) -0.08902(5) 1.13363(8) 0.2081(9) Uani 1 1 d D . .
H26A H 0.3853 -0.0725 1.1870 0.312 Uiso 1 1 calc R . .
H26B H 0.4328 -0.0793 1.1188 0.312 Uiso 1 1 calc R . .
H26C H 0.3497 -0.1414 1.1302 0.312 Uiso 1 1 calc R . .
C27 C 0.35192(12) -0.08402(7) 0.99853(7) 0.3351(13) Uani 1 1 d D . .
H27A H 0.3970 -0.0837 0.9856 0.503 Uiso 1 1 calc R . .
H27B H 0.3421 -0.0568 0.9590 0.503 Uiso 1 1 calc R . .
H27C H 0.3115 -0.1343 1.0001 0.503 Uiso 1 1 calc R . .
C28 C 0.29181(4) -0.04612(7) 1.10799(11) 0.1481(10) Uani 1 1 d D . .
H28A H 0.3023 -0.0222 1.1588 0.222 Uiso 1 1 calc R . .
H28B H 0.2509 -0.0959 1.1128 0.222 Uiso 1 1 calc R . .
H28C H 0.2793 -0.0190 1.0710 0.222 Uiso 1 1 calc R . .
C29 C 0.47609(5) 0.21987(5) 1.20112(5) 0.0831(6) Uani 1 1 d D . .
C30 C 0.53807(7) 0.22444(11) 1.15686(14) 0.3109(12) Uani 1 1 d D . .
H30A H 0.5456 0.1842 1.1719 0.466 Uiso 1 1 calc R . .
H30B H 0.5821 0.2708 1.1682 0.466 Uiso 1 1 calc R . .
H30C H 0.5275 0.2214 1.1012 0.466 Uiso 1 1 calc R . .
C31 C 0.47560(12) 0.28385(9) 1.17016(15) 0.2858(16) Uani 1 1 d D . .
H31A H 0.4397 0.2912 1.1984 0.429 Uiso 1 1 calc R . .
H31B H 0.4628 0.2764 1.1150 0.429 Uiso 1 1 calc R . .
H31C H 0.5240 0.3268 1.1763 0.429 Uiso 1 1 calc R . .
C32 C 0.46856(15) 0.22743(15) 1.28616(8) 0.2941(19) Uani 1 1 d D . .
H32A H 0.4685 0.1870 1.3136 0.441 Uiso 1 1 calc R . .
H32B H 0.4228 0.2267 1.2964 0.441 Uiso 1 1 calc R . .
H32C H 0.5094 0.2736 1.3044 0.441 Uiso 1 1 calc R . .
C33 C 0.18925(3) 0.11228(3) 1.19509(4) 0.0689(4) Uani 1 1 d D . .
C34 C 0.12746(5) 0.09372(9) 1.13393(8) 0.1765(10) Uani 1 1 d D . .
H34A H 0.1152 0.1325 1.1335 0.265 Uiso 1 1 calc R . .
H34B H 0.0842 0.0476 1.1478 0.265 Uiso 1 1 calc R . .
H34C H 0.1444 0.0895 1.0823 0.265 Uiso 1 1 calc R . .
C35 C 0.19127(7) 0.04068(5) 1.17741(17) 0.3316(16) Uani 1 1 d D . .
H35A H 0.2287 0.0394 1.2094 0.497 Uiso 1 1 calc R . .
H35B H 0.2026 0.0397 1.1224 0.497 Uiso 1 1 calc R . .
H35C H 0.1438 -0.0017 1.1893 0.497 Uiso 1 1 calc R . .
C36 C 0.16349(10) 0.11506(16) 1.27902(6) 0.338(2) Uani 1 1 d D . .
H36A H 0.2011 0.1212 1.3162 0.506 Uiso 1 1 calc R . .
H36B H 0.1184 0.0696 1.2902 0.506 Uiso 1 1 calc R . .
H36C H 0.1548 0.1561 1.2835 0.506 Uiso 1 1 calc R . .
C37 C 0.30451(3) 0.38062(4) 1.07533(4) 0.1129(6) Uani 1 1 d D . .
C38 C 0.37335(5) 0.38007(7) 1.09489(18) 0.2669(19) Uani 1 1 d D . .
H38A H 0.3708 0.3636 1.1485 0.400 Uiso 1 1 calc R . .
H38B H 0.4151 0.4293 1.0893 0.400 Uiso 1 1 calc R . .
H38C H 0.3790 0.3470 1.0596 0.400 Uiso 1 1 calc R . .
C39 C 0.28051(6) 0.42013(6) 1.12987(9) 0.2908(11) Uani 1 1 d D . .
H39A H 0.2679 0.3955 1.1803 0.436 Uiso 1 1 calc R . .
H39B H 0.2379 0.4203 1.1082 0.436 Uiso 1 1 calc R . .
H39C H 0.3201 0.4703 1.1366 0.436 Uiso 1 1 calc R . .
C40 C 0.3210(2) 0.41150(12) 0.99384(6) 0.317(3) Uani 1 1 d D . .
H40A H 0.2776 0.4095 0.9717 0.475 Uiso 1 1 calc R . .
H40B H 0.3355 0.3828 0.9616 0.475 Uiso 1 1 calc R . .
H40C H 0.3607 0.4621 0.9955 0.475 Uiso 1 1 calc R . .
C41 C 0.07261(5) 0.18070(6) 0.89544(8) 0.0641(4) Uani 1 1 d . . .
C42 C 0.07136(8) 0.13380(7) 0.82025(11) 0.1190(8) Uani 1 1 d . . .
H42A H 0.1145 0.1283 0.8209 0.178 Uiso 1 1 calc R . .
H42B H 0.0713 0.1592 0.7728 0.178 Uiso 1 1 calc R . .
H42C H 0.0275 0.0857 0.8218 0.178 Uiso 1 1 calc R . .
C43 C 0.07262(7) 0.13360(8) 0.95482(12) 0.1427(8) Uani 1 1 d . . .
H43A H 0.1161 0.1290 0.9496 0.214 Uiso 1 1 calc R . .
H43B H 0.0291 0.0855 0.9497 0.214 Uiso 1 1 calc R . .
H43C H 0.0727 0.1540 1.0058 0.214 Uiso 1 1 calc R . .
C44 C 0.01238(8) 0.20022(10) 0.88258(19) 0.2615(15) Uani 1 1 d . . .
H44A H 0.0254 0.2336 0.8384 0.392 Uiso 1 1 calc R . .
H44B H 0.0074 0.2237 0.9293 0.392 Uiso 1 1 calc R . .
H44C H -0.0338 0.1558 0.8718 0.392 Uiso 1 1 calc R . .
C45 C 0.30493(4) 0.38162(4) 0.71392(4) 0.0996(6) Uani 1 1 d D . .
C46 C 0.33190(14) 0.41288(12) 0.79083(6) 0.2884(18) Uani 1 1 d D . .
H46A H 0.3468 0.3824 0.8191 0.433 Uiso 1 1 calc R . .
H46B H 0.2932 0.4150 0.8197 0.433 Uiso 1 1 calc R . .
H46C H 0.3737 0.4621 0.7852 0.433 Uiso 1 1 calc R . .
C47 C 0.28955(8) 0.41783(7) 0.65068(8) 0.3760(16) Uani 1 1 d D . .
H47A H 0.2454 0.4197 0.6627 0.564 Uiso 1 1 calc R . .
H47B H 0.2824 0.3906 0.6024 0.564 Uiso 1 1 calc R . .
H47C H 0.3306 0.4674 0.6445 0.564 Uiso 1 1 calc R . .
C48 C 0.36891(5) 0.38318(7) 0.68095(13) 0.2412(17) Uani 1 1 d D . .
H48A H 0.3848 0.3570 0.7153 0.362 Uiso 1 1 calc R . .
H48B H 0.4081 0.4338 0.6755 0.362 Uiso 1 1 calc R . .
H48C H 0.3568 0.3598 0.6299 0.362 Uiso 1 1 calc R . .
C49 C 0.18792(4) 0.10891(4) 0.59093(4) 0.1310(7) Uani 1 1 d D . .
C50 C 0.12484(6) 0.10342(11) 0.64298(10) 0.2871(19) Uani 1 1 d D . .
H50A H 0.1171 0.1443 0.6315 0.431 Uiso 1 1 calc R . .
H50B H 0.1379 0.1050 0.6978 0.431 Uiso 1 1 calc R . .
H50C H 0.0801 0.0575 0.6322 0.431 Uiso 1 1 calc R . .
C51 C 0.16350(10) 0.11539(14) 0.50716(6) 0.347(2) Uani 1 1 d D . .
H51A H 0.1683 0.1635 0.5005 0.520 Uiso 1 1 calc R . .
H51B H 0.1126 0.0777 0.4994 0.520 Uiso 1 1 calc R . .
H51C H 0.1942 0.1091 0.4691 0.520 Uiso 1 1 calc R . .
C52 C 0.19508(6) 0.04213(5) 0.61661(15) 0.2432(16) Uani 1 1 d D . .
H52A H 0.2392 0.0460 0.5938 0.365 Uiso 1 1 calc R . .
H52B H 0.1525 -0.0028 0.5988 0.365 Uiso 1 1 calc R . .
H52C H 0.1981 0.0414 0.6733 0.365 Uiso 1 1 calc R . .
C53 C 0.47290(4) 0.21785(4) 0.57659(4) 0.2295(8) Uani 1 1 d D . .
C54 C 0.46988(5) 0.28270(4) 0.61589(6) 0.2295(8) Uani 1 1 d D . .
H54A H 0.4800 0.2835 0.6715 0.344 Uiso 1 1 calc R . .
H54B H 0.4214 0.2767 0.6087 0.344 Uiso 1 1 calc R . .
H54C H 0.5064 0.3285 0.5922 0.344 Uiso 1 1 calc R . .
C55 C 0.46803(6) 0.21875(6) 0.48553(4) 0.2295(8) Uani 1 1 d D . .
H55A H 0.4624 0.1733 0.4645 0.344 Uiso 1 1 calc R . .
H55B H 0.5126 0.2600 0.4649 0.344 Uiso 1 1 calc R . .
H55C H 0.4261 0.2235 0.4705 0.344 Uiso 1 1 calc R . .
C56 C 0.53572(3) 0.20646(5) 0.60764(7) 0.2295(8) Uani 1 1 d D . .
H56A H 0.5352 0.2063 0.6645 0.344 Uiso 1 1 calc R . .
H56B H 0.5825 0.2461 0.5892 0.344 Uiso 1 1 calc R . .
H56C H 0.5288 0.1599 0.5887 0.344 Uiso 1 1 calc R . .
C57 C 0.35879(7) -0.05030(7) 0.71245(10) 0.0971(7) Uani 1 1 d . . .
C58 C 0.29315(8) -0.04803(9) 0.67695(12) 0.1245(9) Uani 1 1 d . . .
H58A H 0.3098 -0.0128 0.6343 0.187 Uiso 1 1 calc R . .
H58B H 0.2701 -0.0335 0.7169 0.187 Uiso 1 1 calc R . .
H58C H 0.2579 -0.0964 0.6572 0.187 Uiso 1 1 calc R . .
C59 C 0.37266(12) -0.09335(10) 0.64957(17) 0.2736(13) Uani 1 1 d . . .
H59A H 0.3762 -0.0711 0.5988 0.410 Uiso 1 1 calc R . .
H59B H 0.3324 -0.1437 0.6491 0.410 Uiso 1 1 calc R . .
H59C H 0.4183 -0.0927 0.6608 0.410 Uiso 1 1 calc R . .
C60 C 0.34877(15) -0.08670(9) 0.78558(14) 0.3246(14) Uani 1 1 d . . .
H60A H 0.3411 -0.0591 0.8265 0.487 Uiso 1 1 calc R . .
H60B H 0.3921 -0.0901 0.7976 0.487 Uiso 1 1 calc R . .
H60C H 0.3062 -0.1357 0.7825 0.487 Uiso 1 1 calc R . .
O2 O 0.0251(3) 0.3054(2) 0.3878(3) 0.637(4) Uani 1 1 d . . .
H2A H 0.0627 0.3218 0.4279 0.765 Uiso 1 1 d R . .
H2B H -0.0107 0.3218 0.3889 0.765 Uiso 1 1 d R . .
O3 O 0.4669(3) 0.4529(3) 0.3640(2) 0.637(4) Uani 1 1 d . . .
H3A H 0.5175 0.4713 0.3484 0.765 Uiso 1 1 d R . .
H3B H 0.4560 0.4713 0.4113 0.765 Uiso 1 1 d R . .
O1 O 0.3437(6) 0.7259(3) 0.5514(4) 0.752(5) Uani 0.33 1 d P . .
H1 H 0.3930 0.7473 0.5726 0.902 Uiso 0.33 1 d PR . .


_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 C53 1.8061(7) . ?
S1 C1 1.8399(9) . ?
S2 C6 1.8114(10) . ?
S2 C57 1.8860(12) . ?
S3 C7 1.8301(11) . ?
S3 C21 1.8382(10) . ?
S4 C8 1.7988(10) . ?
S4 C25 1.8568(7) . ?
S5 C11 1.8358(9) . ?
S5 C29 1.8425(9) . ?
S6 C12 1.8126(9) . ?
S6 C33 1.8474(7) . ?
S7 C37 1.8229(7) . ?
S7 C16 1.8366(10) . ?
S8 C17 1.8153(10) . ?
S8 C41 1.8674(9) . ?
S9 C19 1.8311(11) . ?
S9 C45 1.8348(7) . ?
S10 C20 1.8334(10) . ?
S10 C49 1.8828(7) . ?
C1 C2 1.3369(13) . ?
C1 C6 1.5406(13) . ?
C2 C3 1.3886(15) . ?
C2 C20 1.4258(13) . ?
C3 C4 1.3730(13) . ?
C3 C15 1.3768(13) . ?
C4 C10 1.3666(12) . ?
C4 C5 1.4486(18) . ?
C5 C7 1.3254(14) . ?
C5 C6 1.4262(10) . ?
C7 C8 1.5343(12) . ?
C8 C9 1.4252(13) . ?
C9 C11 1.3378(13) . ?
C9 C10 1.4085(13) . ?
C10 C14 1.3662(13) . ?
C11 C12 1.5182(15) . ?
C12 C13 1.4286(12) . ?
C13 C16 1.3362(14) . ?
C13 C14 1.4193(13) . ?
C14 C15 1.3735(11) . ?
C15 C18 1.4507(17) . ?
C16 C17 1.5283(13) . ?
C17 C18 1.4371(13) . ?
C18 C19 1.3338(11) . ?
C19 C20 1.5307(14) . ?
C21 C24 1.459(2) . ?
C21 C23 1.465(3) . ?
C21 C22 1.584(2) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.5067(16) . ?
C25 C27 1.5116(14) . ?
C25 C28 1.5216(15) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C31 1.434(2) . ?
C29 C30 1.451(2) . ?
C29 C32 1.4612(18) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C36 1.5260(16) . ?
C33 C35 1.5393(16) . ?
C33 C34 1.5396(14) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.4745(16) . ?
C37 C39 1.4771(17) . ?
C37 C40 1.4839(15) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C43 1.402(2) . ?
C41 C44 1.513(3) . ?
C41 C42 1.593(2) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C48 1.4273(17) . ?
C45 C47 1.4317(18) . ?
C45 C46 1.4347(14) . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 C51 1.5310(17) . ?
C49 C52 1.5314(16) . ?
C49 C50 1.5347(17) . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 C56 1.5319(13) . ?
C53 C54 1.5320(13) . ?
C53 C55 1.5412(11) . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 C60 1.408(3) . ?
C57 C59 1.506(3) . ?
C57 C58 1.513(3) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
O2 H2A 0.9601 . ?
O2 H2B 0.9599 . ?
O3 H3A 0.9600 . ?
O3 H3B 0.9599 . ?
O1 H1 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C53 S1 C1 110.50(3) . . ?
C6 S2 C57 101.23(6) . . ?
C7 S3 C21 102.79(5) . . ?
C8 S4 C25 103.44(3) . . ?
C11 S5 C29 105.76(4) . . ?
C12 S6 C33 101.25(3) . . ?
C37 S7 C16 105.05(3) . . ?
C17 S8 C41 101.05(5) . . ?
C19 S9 C45 102.84(4) . . ?
C20 S10 C49 100.34(3) . . ?
C2 C1 C6 122.51(8) . . ?
C2 C1 S1 119.52(7) . . ?
C6 C1 S1 117.97(6) . . ?
C1 C2 C3 109.09(8) . . ?
C1 C2 C20 136.42(10) . . ?
C3 C2 C20 114.48(8) . . ?
C4 C3 C15 105.99(8) . . ?
C4 C3 C2 136.16(9) . . ?
C15 C3 C2 117.85(8) . . ?
C10 C4 C3 109.14(9) . . ?
C10 C4 C5 135.05(9) . . ?
C3 C4 C5 115.81(7) . . ?
C7 C5 C6 138.75(12) . . ?
C7 C5 C4 107.52(7) . . ?
C6 C5 C4 113.71(10) . . ?
C5 C6 C1 122.09(9) . . ?
C5 C6 S2 121.17(8) . . ?
C1 C6 S2 116.74(6) . . ?
C5 C7 C8 123.88(9) . . ?
C5 C7 S3 118.07(8) . . ?
C8 C7 S3 117.98(6) . . ?
C9 C8 C7 120.65(8) . . ?
C9 C8 S4 123.02(7) . . ?
C7 C8 S4 116.33(7) . . ?
C11 C9 C10 107.44(9) . . ?
C11 C9 C8 136.58(9) . . ?
C10 C9 C8 115.86(8) . . ?
C14 C10 C4 108.37(8) . . ?
C14 C10 C9 135.78(8) . . ?
C4 C10 C9 115.86(9) . . ?
C9 C11 C12 123.99(8) . . ?
C9 C11 S5 119.58(8) . . ?
C12 C11 S5 116.41(5) . . ?
C13 C12 C11 122.13(7) . . ?
C13 C12 S6 118.98(8) . . ?
C11 C12 S6 118.89(6) . . ?
C16 C13 C14 106.27(8) . . ?
C16 C13 C12 140.08(9) . . ?
C14 C13 C12 113.65(9) . . ?
C10 C14 C15 106.89(8) . . ?
C10 C14 C13 116.83(8) . . ?
C15 C14 C13 136.28(9) . . ?
C14 C15 C3 109.59(9) . . ?
C14 C15 C18 116.90(8) . . ?
C3 C15 C18 133.50(7) . . ?
C13 C16 C17 125.39(8) . . ?
C13 C16 S7 118.49(7) . . ?
C17 C16 S7 116.01(7) . . ?
C18 C17 C16 121.81(8) . . ?
C18 C17 S8 120.71(7) . . ?
C16 C17 S8 117.34(6) . . ?
C19 C18 C17 139.13(11) . . ?
C19 C18 C15 108.22(9) . . ?
C17 C18 C15 112.45(7) . . ?
C18 C19 C20 122.93(10) . . ?
C18 C19 S9 117.44(9) . . ?
C20 C19 S9 119.60(6) . . ?
C2 C20 C19 122.55(8) . . ?
C2 C20 S10 122.73(7) . . ?
C19 C20 S10 114.66(7) . . ?
C24 C21 C23 111.58(16) . . ?
C24 C21 C22 93.00(16) . . ?
C23 C21 C22 115.46(16) . . ?
C24 C21 S3 107.74(9) . . ?
C23 C21 S3 115.12(11) . . ?
C22 C21 S3 111.58(10) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C27 104.97(11) . . ?
C26 C25 C28 113.07(9) . . ?
C27 C25 C28 115.53(12) . . ?
C26 C25 S4 104.08(5) . . ?
C27 C25 S4 105.17(6) . . ?
C28 C25 S4 112.96(6) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 C29 C30 99.76(14) . . ?
C31 C29 C32 101.97(18) . . ?
C30 C29 C32 129.66(17) . . ?
C31 C29 S5 111.59(10) . . ?
C30 C29 S5 112.49(9) . . ?
C32 C29 S5 100.62(10) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C36 C33 C35 113.36(16) . . ?
C36 C33 C34 111.56(10) . . ?
C35 C33 C34 92.89(11) . . ?
C36 C33 S6 106.06(8) . . ?
C35 C33 S6 115.80(7) . . ?
C34 C33 S6 117.11(7) . . ?
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 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C39 117.64(13) . . ?
C38 C37 C40 101.3(2) . . ?
C39 C37 C40 114.00(16) . . ?
C38 C37 S7 112.47(7) . . ?
C39 C37 S7 104.25(5) . . ?
C40 C37 S7 107.02(9) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C43 C41 C44 125.42(14) . . ?
C43 C41 C42 98.50(13) . . ?
C44 C41 C42 106.72(15) . . ?
C43 C41 S8 113.93(8) . . ?
C44 C41 S8 102.40(9) . . ?
C42 C41 S8 109.02(8) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C48 C45 C47 98.51(11) . . ?
C48 C45 C46 101.18(15) . . ?
C47 C45 C46 125.18(14) . . ?
C48 C45 S9 112.24(8) . . ?
C47 C45 S9 104.52(6) . . ?
C46 C45 S9 113.95(8) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C48 H48A 109.5 . . ?
C45 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C45 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C51 C49 C52 121.87(15) . . ?
C51 C49 C50 103.11(12) . . ?
C52 C49 C50 103.73(12) . . ?
C51 C49 S10 102.99(8) . . ?
C52 C49 S10 111.84(6) . . ?
C50 C49 S10 113.28(8) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C49 C52 H52A 109.5 . . ?
C49 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C49 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C56 C53 C54 113.65(7) . . ?
C56 C53 C55 114.17(8) . . ?
C54 C53 C55 112.92(8) . . ?
C56 C53 S1 105.33(5) . . ?
C54 C53 S1 106.00(6) . . ?
C55 C53 S1 103.54(5) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C60 C57 C59 108.62(18) . . ?
C60 C57 C58 118.08(17) . . ?
C59 C57 C58 100.55(16) . . ?
C60 C57 S2 110.57(12) . . ?
C59 C57 S2 107.01(10) . . ?
C58 C57 S2 111.00(11) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
H2A O2 H2B 120.0 . . ?
H3A O3 H3B 120.0 . . ?

loop_
# start Validation Reply Form
_vrf_PLAT213_Keinan-58
;
PROBLEM: Atom C32 has ADP max/min Ratio ...6.30 prola
RESPONSE: Partly disordered tert-butyl group
;
_vrf_PLAT214_Keinan-58           
;
PROBLEM: Atom O1 (Anion/Solvent) ADP max/min Ratio 8.50 prola
RESPONSE: Disordered water molecule
;
_vrf_PLAT220_Keinan-58           
;
PROBLEM: Large Non-Solvent C  Ueq(max)/Ueq(min) ...6.34 Ratio
RESPONSE: Partly disordered tert-butyl group
;
_vrf_PLAT241_Keinan-58           
;
PROBLEM: Check High Ueq as Compared to Neighbors for  C12     
RESPONSE: Central core of the main molecule  is disordered
;
_vrf_PLAT242_Keinan-58           
;
PROBLEM: Check Low Ueq as Compared to Neighbors for S1     
RESPONSE: 'S-atoms are connected to the disordered central core of the 
main molecule'
;
_vrf_PLAT602_Keinan-58           
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure !
RESPONSE: Three are unresolved solvents at the crystal structure
;
_vrf_PLAT230_Keinan-58           
;
PROBLEM: Hirshfeld Test Diff for S3 -- C7 .. 163.07 su   
RESPONSE: 'S-atoms are connected to the disordered central core of the 
main molecule'
;
# end Validation Reply Form

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.73
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.121
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Mix of hexane-THF'
