# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1838111'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 O4 S2 W'
_chemical_formula_sum            'C30 H44 O4 S2 W'
_chemical_formula_weight         716.62

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'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   12.4416(16)
_cell_length_b                   14.4457(18)
_cell_length_c                   17.920(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3220.7(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3159
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      23.52

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_F_000             1448
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    3.747
_shelx_estimated_absorpt_T_min   0.467
_shelx_estimated_absorpt_T_max   0.662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.437
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'Sadabs Bruker'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         microsource
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26945
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.811
_diffrn_reflns_theta_max         25.556
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6007
_reflns_number_gt                5364
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'Bruker SMART (2001)'
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Diamond (Brandenburg)'

_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)+(0.0303P)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_abs_structure_details 
;
 Flack x determined using 2141 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.016(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6007
_refine_ls_number_parameters     347
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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_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
W1 W 0.45722(3) 0.02667(2) 0.34786(2) 0.01774(10) Uani 1 1 d . . . . .
S1 S 0.42372(19) -0.14852(17) 0.29725(14) 0.0232(6) Uani 1 1 d . . . . .
S2 S 0.61954(19) 0.00461(16) 0.24851(14) 0.0252(6) Uani 1 1 d . . . . .
O1 O 0.3785(5) 0.0416(4) 0.2550(3) 0.0202(14) Uani 1 1 d . . . . .
O2 O 0.5702(4) -0.0350(5) 0.4039(3) 0.0238(15) Uani 1 1 d . . . . .
O3 O 0.4943(5) 0.1390(5) 0.3554(4) 0.0279(16) Uani 1 1 d . . . . .
O4 O 0.3564(5) 0.0075(4) 0.4117(3) 0.0245(17) Uani 1 1 d . . . . .
C1 C 0.3329(6) -0.0202(7) 0.2079(5) 0.0167(18) Uani 1 1 d . . . . .
C2 C 0.3432(7) -0.1131(7) 0.2212(5) 0.022(2) Uani 1 1 d . . . . .
C3 C 0.2969(7) -0.1787(6) 0.1733(5) 0.020(2) Uani 1 1 d . . . . .
H3 H 0.3050 -0.2428 0.1836 0.024 Uiso 1 1 calc R U . . .
C4 C 0.2397(7) -0.1508(7) 0.1110(5) 0.019(2) Uani 1 1 d . . . . .
C5 C 0.2339(7) -0.0553(6) 0.0981(5) 0.021(2) Uani 1 1 d . . . . .
H5 H 0.1973 -0.0355 0.0543 0.025 Uiso 1 1 calc R U . . .
C6 C 0.2767(6) 0.0122(6) 0.1433(5) 0.019(2) Uani 1 1 d . . . . .
C7 C 0.1876(8) -0.2206(7) 0.0568(6) 0.026(2) Uani 1 1 d . . . . .
C8 C 0.0690(7) -0.1945(8) 0.0465(6) 0.033(3) Uani 1 1 d . . . . .
H8A H 0.0367 -0.2344 0.0083 0.049 Uiso 1 1 calc R U . . .
H8B H 0.0638 -0.1297 0.0306 0.049 Uiso 1 1 calc R U . . .
H8C H 0.0307 -0.2027 0.0938 0.049 Uiso 1 1 calc R U . . .
C9 C 0.1942(9) -0.3184(7) 0.0858(6) 0.037(3) Uani 1 1 d . . . . .
H9A H 0.1638 -0.3210 0.1362 0.056 Uiso 1 1 calc R U . . .
H9B H 0.2695 -0.3381 0.0873 0.056 Uiso 1 1 calc R U . . .
H9C H 0.1535 -0.3596 0.0528 0.056 Uiso 1 1 calc R U . . .
C10 C 0.2448(9) -0.2136(8) -0.0186(6) 0.033(3) Uani 1 1 d . . . . .
H10A H 0.3214 -0.2272 -0.0120 0.049 Uiso 1 1 calc R U . . .
H10B H 0.2364 -0.1508 -0.0385 0.049 Uiso 1 1 calc R U . . .
H10C H 0.2133 -0.2582 -0.0534 0.049 Uiso 1 1 calc R U . . .
C11 C 0.2697(8) 0.1153(7) 0.1262(6) 0.023(2) Uani 1 1 d . . . . .
C12 C 0.3856(8) 0.1501(7) 0.1110(5) 0.027(2) Uani 1 1 d . . . . .
H12A H 0.4304 0.1387 0.1550 0.040 Uiso 1 1 calc R U . . .
H12B H 0.3839 0.2166 0.1003 0.040 Uiso 1 1 calc R U . . .
H12C H 0.4156 0.1170 0.0681 0.040 Uiso 1 1 calc R U . . .
C13 C 0.2033(9) 0.1344(7) 0.0560(7) 0.033(3) Uani 1 1 d . . . . .
H13A H 0.2359 0.1026 0.0133 0.050 Uiso 1 1 calc R U . . .
H13B H 0.2016 0.2011 0.0464 0.050 Uiso 1 1 calc R U . . .
H13C H 0.1298 0.1116 0.0633 0.050 Uiso 1 1 calc R U . . .
C14 C 0.2190(8) 0.1701(7) 0.1896(6) 0.027(2) Uani 1 1 d . . . . .
H14A H 0.1468 0.1459 0.1998 0.041 Uiso 1 1 calc R U . . .
H14B H 0.2139 0.2354 0.1754 0.041 Uiso 1 1 calc R U . . .
H14C H 0.2635 0.1642 0.2345 0.041 Uiso 1 1 calc R U . . .
C15 C 0.5483(8) -0.1778(6) 0.2498(6) 0.030(2) Uani 1 1 d . . . . .
H15A H 0.6033 -0.1930 0.2877 0.036 Uiso 1 1 calc R U . . .
H15B H 0.5362 -0.2340 0.2193 0.036 Uiso 1 1 calc R U . . .
C16 C 0.5914(9) -0.1033(8) 0.2005(6) 0.037(3) Uani 1 1 d . . . . .
H16A H 0.5387 -0.0911 0.1602 0.044 Uiso 1 1 calc R U . . .
H16B H 0.6584 -0.1256 0.1767 0.044 Uiso 1 1 calc R U . . .
C17 C 0.7134(7) -0.0306(8) 0.3166(5) 0.021(2) Uani 1 1 d . . . . .
C18 C 0.6778(7) -0.0444(7) 0.3891(5) 0.019(2) Uani 1 1 d . . . . .
C19 C 0.7489(7) -0.0691(6) 0.4457(5) 0.019(2) Uani 1 1 d . . . . .
C20 C 0.8560(8) -0.0759(7) 0.4251(5) 0.022(2) Uani 1 1 d . . . . .
H20 H 0.9063 -0.0924 0.4627 0.026 Uiso 1 1 calc R U . . .
C21 C 0.8960(7) -0.0602(6) 0.3526(6) 0.022(2) Uani 1 1 d . . . . .
C22 C 0.8220(7) -0.0384(7) 0.2982(5) 0.023(2) Uani 1 1 d . . . . .
H22 H 0.8448 -0.0287 0.2482 0.027 Uiso 1 1 calc R U . . .
C23 C 1.0158(7) -0.0662(8) 0.3366(7) 0.033(3) Uani 1 1 d . . . . .
C24A C 1.0383(13) -0.0501(9) 0.2519(8) 0.032(4) Uiso 0.724(15) 1 d . . P A 1
H24A H 1.0031 -0.0988 0.2226 0.048 Uiso 0.724(15) 1 calc R U P A 1
H24B H 1.1160 -0.0519 0.2428 0.048 Uiso 0.724(15) 1 calc R U P A 1
H24C H 1.0100 0.0104 0.2369 0.048 Uiso 0.724(15) 1 calc R U P A 1
C25A C 1.0600(13) -0.1558(10) 0.3620(9) 0.042(5) Uiso 0.724(15) 1 d . . P A 1
H25A H 1.0487 -0.1622 0.4159 0.063 Uiso 0.724(15) 1 calc R U P A 1
H25B H 1.1371 -0.1581 0.3511 0.063 Uiso 0.724(15) 1 calc R U P A 1
H25C H 1.0235 -0.2064 0.3359 0.063 Uiso 0.724(15) 1 calc R U P A 1
C26A C 1.0725(13) 0.0140(12) 0.3782(9) 0.046(5) Uiso 0.724(15) 1 d . . P A 1
H26A H 1.0505 0.0138 0.4307 0.069 Uiso 0.724(15) 1 calc R U P A 1
H26B H 1.0524 0.0731 0.3552 0.069 Uiso 0.724(15) 1 calc R U P A 1
H26C H 1.1506 0.0057 0.3750 0.069 Uiso 0.724(15) 1 calc R U P A 1
C24B C 1.057(4) 0.007(3) 0.287(3) 0.061(15) Uiso 0.276(15) 1 d . . P A 2
H24D H 1.0249 0.0008 0.2376 0.091 Uiso 0.276(15) 1 calc R U P A 2
H24E H 1.1354 0.0020 0.2832 0.091 Uiso 0.276(15) 1 calc R U P A 2
H24F H 1.0385 0.0680 0.3079 0.091 Uiso 0.276(15) 1 calc R U P A 2
C25B C 1.028(4) -0.160(3) 0.283(3) 0.058(14) Uiso 0.276(15) 1 d . . P A 2
H25D H 1.1039 -0.1687 0.2694 0.086 Uiso 0.276(15) 1 calc R U P A 2
H25E H 0.9850 -0.1527 0.2378 0.086 Uiso 0.276(15) 1 calc R U P A 2
H25F H 1.0031 -0.2147 0.3108 0.086 Uiso 0.276(15) 1 calc R U P A 2
C26B C 1.084(3) -0.086(3) 0.400(2) 0.040(12) Uiso 0.276(15) 1 d . . P A 2
H26D H 1.1553 -0.1054 0.3825 0.060 Uiso 0.276(15) 1 calc R U P A 2
H26E H 1.0521 -0.1355 0.4301 0.060 Uiso 0.276(15) 1 calc R U P A 2
H26F H 1.0916 -0.0300 0.4308 0.060 Uiso 0.276(15) 1 calc R U P A 2
C27 C 0.7126(8) -0.0804(7) 0.5275(5) 0.022(2) Uani 1 1 d . . . . .
C28 C 0.6209(9) -0.1512(8) 0.5333(6) 0.031(3) Uani 1 1 d . . . . .
H28A H 0.5623 -0.1330 0.4998 0.046 Uiso 1 1 calc R U . . .
H28B H 0.5943 -0.1531 0.5848 0.046 Uiso 1 1 calc R U . . .
H28C H 0.6474 -0.2125 0.5190 0.046 Uiso 1 1 calc R U . . .
C29 C 0.8035(8) -0.1164(7) 0.5763(5) 0.028(3) Uani 1 1 d . . . . .
H29A H 0.7762 -0.1286 0.6267 0.041 Uiso 1 1 calc R U . . .
H29B H 0.8608 -0.0699 0.5788 0.041 Uiso 1 1 calc R U . . .
H29C H 0.8320 -0.1738 0.5549 0.041 Uiso 1 1 calc R U . . .
C30 C 0.6753(8) 0.0132(8) 0.5558(6) 0.031(2) Uani 1 1 d . . . . .
H30A H 0.6167 0.0360 0.5241 0.047 Uiso 1 1 calc R U . . .
H30B H 0.7353 0.0571 0.5542 0.047 Uiso 1 1 calc R U . . .
H30C H 0.6497 0.0071 0.6072 0.047 Uiso 1 1 calc R 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
W1 O3 1.693(7) . ?
W1 O4 1.720(6) . ?
W1 O1 1.942(6) . ?
W1 O2 1.944(6) . ?
W1 S2 2.711(2) . ?
W1 S1 2.720(3) . ?
S1 C2 1.767(10) . ?
S1 C15 1.818(10) . ?
S2 C17 1.763(9) . ?
S2 C16 1.815(12) . ?
O1 C1 1.354(10) . ?
O2 C18 1.371(10) . ?
C1 C2 1.368(13) . ?
C1 C6 1.433(12) . ?
C2 C3 1.402(13) . ?
C3 C4 1.383(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(13) . ?
C4 C7 1.543(13) . ?
C5 C6 1.375(12) . ?
C5 H5 0.9500 . ?
C6 C11 1.522(12) . ?
C7 C9 1.507(14) . ?
C7 C10 1.530(14) . ?
C7 C8 1.535(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C14 1.523(13) . ?
C11 C13 1.531(14) . ?
C11 C12 1.551(13) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.492(15) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.389(12) . ?
C17 C22 1.395(12) . ?
C18 C19 1.392(13) . ?
C19 C20 1.387(12) . ?
C19 C27 1.542(13) . ?
C20 C21 1.409(14) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(13) . ?
C21 C23 1.520(12) . ?
C22 H22 0.9500 . ?
C23 C26B 1.45(4) . ?
C23 C24B 1.48(5) . ?
C23 C25A 1.479(17) . ?
C23 C26A 1.547(18) . ?
C23 C24A 1.562(18) . ?
C23 C25B 1.67(5) . ?
C24A H24A 0.9800 . ?
C24A H24B 0.9800 . ?
C24A H24C 0.9800 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C24B H24D 0.9800 . ?
C24B H24E 0.9800 . ?
C24B H24F 0.9800 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
C27 C30 1.518(13) . ?
C27 C29 1.521(13) . ?
C27 C28 1.536(14) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 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
O3 W1 O4 107.5(3) . . ?
O3 W1 O1 95.7(3) . . ?
O4 W1 O1 102.7(3) . . ?
O3 W1 O2 101.6(3) . . ?
O4 W1 O2 96.3(3) . . ?
O1 W1 O2 149.1(3) . . ?
O3 W1 S2 87.8(2) . . ?
O4 W1 S2 164.0(2) . . ?
O1 W1 S2 79.98(18) . . ?
O2 W1 S2 75.32(18) . . ?
O3 W1 S1 163.8(2) . . ?
O4 W1 S1 87.7(2) . . ?
O1 W1 S1 74.98(18) . . ?
O2 W1 S1 81.8(2) . . ?
S2 W1 S1 77.64(7) . . ?
C2 S1 C15 101.0(5) . . ?
C2 S1 W1 94.3(3) . . ?
C15 S1 W1 104.0(3) . . ?
C17 S2 C16 102.0(5) . . ?
C17 S2 W1 94.2(3) . . ?
C16 S2 W1 105.6(4) . . ?
C1 O1 W1 132.2(6) . . ?
C18 O2 W1 130.7(6) . . ?
O1 C1 C2 120.0(8) . . ?
O1 C1 C6 119.5(9) . . ?
C2 C1 C6 120.5(8) . . ?
C1 C2 C3 121.1(9) . . ?
C1 C2 S1 118.1(7) . . ?
C3 C2 S1 120.6(7) . . ?
C4 C3 C2 120.6(9) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 116.6(9) . . ?
C3 C4 C7 122.2(9) . . ?
C5 C4 C7 121.2(8) . . ?
C6 C5 C4 125.5(9) . . ?
C6 C5 H5 117.2 . . ?
C4 C5 H5 117.2 . . ?
C5 C6 C1 115.7(8) . . ?
C5 C6 C11 123.6(8) . . ?
C1 C6 C11 120.7(8) . . ?
C9 C7 C10 110.0(9) . . ?
C9 C7 C8 108.9(8) . . ?
C10 C7 C8 108.9(9) . . ?
C9 C7 C4 111.9(8) . . ?
C10 C7 C4 108.5(8) . . ?
C8 C7 C4 108.6(8) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C6 C11 C14 112.5(8) . . ?
C6 C11 C13 111.9(8) . . ?
C14 C11 C13 107.2(8) . . ?
C6 C11 C12 107.4(8) . . ?
C14 C11 C12 110.3(8) . . ?
C13 C11 C12 107.4(9) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 S1 114.6(7) . . ?
C16 C15 H15A 108.6 . . ?
S1 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
S1 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 S2 114.1(7) . . ?
C15 C16 H16A 108.7 . . ?
S2 C16 H16A 108.7 . . ?
C15 C16 H16B 108.7 . . ?
S2 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C22 121.3(8) . . ?
C18 C17 S2 118.5(7) . . ?
C22 C17 S2 120.1(7) . . ?
O2 C18 C17 118.6(8) . . ?
O2 C18 C19 120.3(8) . . ?
C17 C18 C19 121.1(8) . . ?
C20 C19 C18 115.8(9) . . ?
C20 C19 C27 121.8(8) . . ?
C18 C19 C27 122.2(8) . . ?
C19 C20 C21 125.0(9) . . ?
C19 C20 H20 117.5 . . ?
C21 C20 H20 117.5 . . ?
C22 C21 C20 117.0(8) . . ?
C22 C21 C23 122.3(11) . . ?
C20 C21 C23 120.7(10) . . ?
C21 C22 C17 119.9(9) . . ?
C21 C22 H22 120.1 . . ?
C17 C22 H22 120.1 . . ?
C26B C23 C24B 114(3) . . ?
C26B C23 C21 116.0(19) . . ?
C24B C23 C21 114(2) . . ?
C25A C23 C21 110.9(10) . . ?
C25A C23 C26A 109.7(11) . . ?
C21 C23 C26A 108.3(10) . . ?
C25A C23 C24A 111.3(11) . . ?
C21 C23 C24A 110.6(11) . . ?
C26A C23 C24A 106.0(10) . . ?
C26B C23 C25B 104(3) . . ?
C24B C23 C25B 102(3) . . ?
C21 C23 C25B 104(2) . . ?
C23 C24A H24A 109.5 . . ?
C23 C24A H24B 109.5 . . ?
H24A C24A H24B 109.5 . . ?
C23 C24A H24C 109.5 . . ?
H24A C24A H24C 109.5 . . ?
H24B C24A H24C 109.5 . . ?
C23 C25A H25A 109.5 . . ?
C23 C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
C23 C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C23 C26A H26A 109.5 . . ?
C23 C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C23 C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C23 C24B H24D 109.5 . . ?
C23 C24B H24E 109.5 . . ?
H24D C24B H24E 109.5 . . ?
C23 C24B H24F 109.5 . . ?
H24D C24B H24F 109.5 . . ?
H24E C24B H24F 109.5 . . ?
C23 C25B H25D 109.5 . . ?
C23 C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C23 C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C23 C26B H26D 109.5 . . ?
C23 C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C23 C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C30 C27 C29 109.9(8) . . ?
C30 C27 C28 110.1(8) . . ?
C29 C27 C28 106.6(8) . . ?
C30 C27 C19 108.2(8) . . ?
C29 C27 C19 111.4(8) . . ?
C28 C27 C19 110.7(8) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 O1 C1 C2 -3.4(12) . . . . ?
W1 O1 C1 C6 178.4(6) . . . . ?
O1 C1 C2 C3 -179.8(8) . . . . ?
C6 C1 C2 C3 -1.6(14) . . . . ?
O1 C1 C2 S1 -3.8(12) . . . . ?
C6 C1 C2 S1 174.4(6) . . . . ?
C15 S1 C2 C1 -99.1(8) . . . . ?
W1 S1 C2 C1 6.1(8) . . . . ?
C15 S1 C2 C3 76.9(8) . . . . ?
W1 S1 C2 C3 -177.9(7) . . . . ?
C1 C2 C3 C4 0.1(14) . . . . ?
S1 C2 C3 C4 -175.8(7) . . . . ?
C2 C3 C4 C5 1.9(13) . . . . ?
C2 C3 C4 C7 180.0(9) . . . . ?
C3 C4 C5 C6 -2.5(14) . . . . ?
C7 C4 C5 C6 179.3(9) . . . . ?
C4 C5 C6 C1 1.1(13) . . . . ?
C4 C5 C6 C11 179.1(8) . . . . ?
O1 C1 C6 C5 179.3(8) . . . . ?
C2 C1 C6 C5 1.1(12) . . . . ?
O1 C1 C6 C11 1.2(12) . . . . ?
C2 C1 C6 C11 -177.0(8) . . . . ?
C3 C4 C7 C9 7.8(13) . . . . ?
C5 C4 C7 C9 -174.2(9) . . . . ?
C3 C4 C7 C10 -113.7(10) . . . . ?
C5 C4 C7 C10 64.3(11) . . . . ?
C3 C4 C7 C8 128.0(10) . . . . ?
C5 C4 C7 C8 -54.0(12) . . . . ?
C5 C6 C11 C14 124.6(9) . . . . ?
C1 C6 C11 C14 -57.5(11) . . . . ?
C5 C6 C11 C13 3.8(13) . . . . ?
C1 C6 C11 C13 -178.3(8) . . . . ?
C5 C6 C11 C12 -113.8(10) . . . . ?
C1 C6 C11 C12 64.1(10) . . . . ?
C2 S1 C15 C16 52.7(8) . . . . ?
W1 S1 C15 C16 -44.5(8) . . . . ?
S1 C15 C16 S2 59.1(9) . . . . ?
C17 S2 C16 C15 58.6(8) . . . . ?
W1 S2 C16 C15 -39.2(8) . . . . ?
C16 S2 C17 C18 -100.7(9) . . . . ?
W1 S2 C17 C18 6.2(9) . . . . ?
C16 S2 C17 C22 83.3(10) . . . . ?
W1 S2 C17 C22 -169.8(9) . . . . ?
W1 O2 C18 C17 -18.8(14) . . . . ?
W1 O2 C18 C19 162.4(7) . . . . ?
C22 C17 C18 O2 179.5(9) . . . . ?
S2 C17 C18 O2 3.5(14) . . . . ?
C22 C17 C18 C19 -1.8(17) . . . . ?
S2 C17 C18 C19 -177.8(7) . . . . ?
O2 C18 C19 C20 -179.4(9) . . . . ?
C17 C18 C19 C20 1.8(14) . . . . ?
O2 C18 C19 C27 -4.2(14) . . . . ?
C17 C18 C19 C27 177.1(9) . . . . ?
C18 C19 C20 C21 -0.2(14) . . . . ?
C27 C19 C20 C21 -175.5(9) . . . . ?
C19 C20 C21 C22 -1.5(15) . . . . ?
C19 C20 C21 C23 177.8(9) . . . . ?
C20 C21 C22 C17 1.5(14) . . . . ?
C23 C21 C22 C17 -177.7(10) . . . . ?
C18 C17 C22 C21 0.0(16) . . . . ?
S2 C17 C22 C21 175.9(8) . . . . ?
C22 C21 C23 C26B 177(2) . . . . ?
C20 C21 C23 C26B -2(2) . . . . ?
C22 C21 C23 C24B 41(3) . . . . ?
C20 C21 C23 C24B -138(2) . . . . ?
C22 C21 C23 C25A -127.1(12) . . . . ?
C20 C21 C23 C25A 53.7(15) . . . . ?
C22 C21 C23 C26A 112.5(12) . . . . ?
C20 C21 C23 C26A -66.7(13) . . . . ?
C22 C21 C23 C24A -3.2(14) . . . . ?
C20 C21 C23 C24A 177.6(9) . . . . ?
C22 C21 C23 C25B -69(2) . . . . ?
C20 C21 C23 C25B 111(2) . . . . ?
C20 C19 C27 C30 110.5(10) . . . . ?
C18 C19 C27 C30 -64.5(11) . . . . ?
C20 C19 C27 C29 -10.4(13) . . . . ?
C18 C19 C27 C29 174.6(9) . . . . ?
C20 C19 C27 C28 -128.9(10) . . . . ?
C18 C19 C27 C28 56.1(12) . . . . ?

_refine_diff_density_max         2.135
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.125

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1853496'
_audit_update_record             
;
2018-07-04 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C34 H50 O4 S2 W [+ solvent]'
_chemical_formula_sum            'C34 H50 O4 S2 W [+ solvent]'
_chemical_formula_weight         770.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 '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                   21.333(3)
_cell_length_b                   21.333(3)
_cell_length_c                   45.902(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     18091(6)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25511
_cell_measurement_theta_min      4.14
_cell_measurement_theta_max      60.23

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_F_000             7056
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    6.522
_shelx_estimated_absorpt_T_min   0.484
_shelx_estimated_absorpt_T_max   0.534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9683
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_process_details   'STOE X-Red32'

_exptl_special_details           
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.

;


_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Counting Detector'
_diffrn_detector_type            'Dectris Pilatus 200K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'Xenocs Cu microfocus tube'
_diffrn_radiation_probe          x-ray
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_measurement_device       '4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 2026 frames, detector distance = 60 mm
;
_diffrn_reflns_number            20555
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         4.536
_diffrn_reflns_theta_max         60.221
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measured_fraction_theta_full 0.784
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_Laue_measured_fraction_full 0.784
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_point_group_measured_fraction_full 0.784
_reflns_number_total             5730
_reflns_number_gt                3410
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.131.0 (STOE, 2017)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.71.0.0 (STOE, 2016)
X-Area LANA 1.71.4.0 (STOE, 2017)
;
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;

_computing_molecular_graphics    'DIAMOND (Brandenburg, 2018)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1131P)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         5730
_refine_ls_number_parameters     364
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1957
_refine_ls_wR_factor_gt          0.1701
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_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
W1 W 0.84251(3) 0.09188(3) 0.81230(2) 0.1003(3) Uani 1 1 d . . . . .
S1 S 0.95771(13) 0.07837(13) 0.79899(5) 0.0885(6) Uani 1 1 d . . . . .
S2 S 0.93789(16) 0.20422(15) 0.83870(6) 0.1050(8) Uani 1 1 d . . . . .
O1 O 0.8788(4) 0.1492(4) 0.77664(16) 0.111(2) Uani 1 1 d . . . . .
O2 O 0.8532(3) 0.0532(4) 0.85033(14) 0.0944(17) Uani 1 1 d . . . . .
O3 O 0.7861(4) -0.0059(5) 0.79617(15) 0.118(2) Uani 1 1 d . . . . .
O4 O 0.6824(5) -0.1017(7) 0.7858(3) 0.177(4) Uani 1 1 d . . . . .
C1 C 0.9328(6) 0.1566(6) 0.7591(2) 0.100(3) Uani 1 1 d . . . . .
C2 C 0.9794(6) 0.1303(6) 0.7667(2) 0.094(3) Uani 1 1 d . . . . .
C3 C 1.0340(6) 0.1369(6) 0.7488(2) 0.101(3) Uani 1 1 d . . . . .
H3 H 1.0628 0.1165 0.7545 0.122 Uiso 1 1 calc R U . . .
C4 C 1.0472(6) 0.1732(6) 0.7225(2) 0.105(3) Uani 1 1 d . . . . .
C5 C 1.0021(7) 0.2014(6) 0.7153(2) 0.111(3) Uani 1 1 d . . . . .
H5 H 1.0116 0.2273 0.6975 0.133 Uiso 1 1 calc R U . . .
C6 C 0.9449(7) 0.1946(6) 0.7320(2) 0.108(3) Uani 1 1 d . . . . .
C7 C 1.1080(8) 0.1824(7) 0.7020(2) 0.127(4) Uani 1 1 d . . . . .
C8A C 1.1560(12) 0.1553(12) 0.7143(4) 0.089(7) Uiso 0.47(2) 1 d . . P A 1
H8A H 1.1259 0.1068 0.7224 0.134 Uiso 0.47(2) 1 calc R U P A 1
H8B H 1.1868 0.1882 0.7296 0.134 Uiso 0.47(2) 1 calc R U P A 1
H8C H 1.1864 0.1534 0.6987 0.134 Uiso 0.47(2) 1 calc R U P A 1
C9A C 1.139(3) 0.254(2) 0.6867(10) 0.184(16) Uiso 0.47(2) 1 d . . P A 1
H9A H 1.1611 0.2514 0.6682 0.276 Uiso 0.47(2) 1 calc R U P A 1
H9B H 1.1763 0.2918 0.6990 0.276 Uiso 0.47(2) 1 calc R U P A 1
H9C H 1.1007 0.2650 0.6827 0.276 Uiso 0.47(2) 1 calc R U P A 1
C8B C 1.108(3) 0.113(3) 0.7035(10) 0.219(18) Uiso 0.53(2) 1 d . . P A 2
H8D H 1.1524 0.1208 0.7127 0.328 Uiso 0.53(2) 1 calc R U P A 2
H8E H 1.1040 0.0939 0.6838 0.328 Uiso 0.53(2) 1 calc R U P A 2
H8F H 1.0660 0.0782 0.7151 0.328 Uiso 0.53(2) 1 calc R U P A 2
C9B C 1.1660(16) 0.2612(15) 0.7014(7) 0.134(9) Uiso 0.53(2) 1 d . . P A 2
H9D H 1.1959 0.2729 0.7190 0.201 Uiso 0.53(2) 1 calc R U P A 2
H9E H 1.1433 0.2914 0.7007 0.201 Uiso 0.53(2) 1 calc R U P A 2
H9F H 1.1964 0.2706 0.6841 0.201 Uiso 0.53(2) 1 calc R U P A 2
C10 C 1.0742(12) 0.1514(12) 0.6718(4) 0.208(8) Uani 1 1 d . . . . .
H10A H 1.0213 0.1247 0.6735 0.312 Uiso 0.47(2) 1 calc R U P A 1
H10B H 1.0909 0.1188 0.6650 0.312 Uiso 0.47(2) 1 calc R U P A 1
H10C H 1.0890 0.1913 0.6579 0.312 Uiso 0.47(2) 1 calc R U P A 1
H10D H 1.1129 0.1648 0.6575 0.312 Uiso 0.53(2) 1 calc R U P A 2
H10E H 1.0436 0.1714 0.6659 0.312 Uiso 0.53(2) 1 calc R U P A 2
H10F H 1.0448 0.0986 0.6730 0.312 Uiso 0.53(2) 1 calc R U P A 2
C11 C 0.8953(8) 0.2253(8) 0.7233(3) 0.126(4) Uani 1 1 d . . . . .
C12 C 0.9218(9) 0.2655(9) 0.6930(3) 0.164(6) Uani 1 1 d . . . . .
H12A H 0.9154 0.2304 0.6779 0.246 Uiso 1 1 calc R U . . .
H12B H 0.9731 0.3025 0.6944 0.246 Uiso 1 1 calc R U . . .
H12C H 0.8933 0.2885 0.6880 0.246 Uiso 1 1 calc R U . . .
C13 C 0.8189(8) 0.1645(9) 0.7202(3) 0.158(6) Uani 1 1 d . . . . .
H13A H 0.8022 0.1391 0.7389 0.237 Uiso 1 1 calc R U . . .
H13B H 0.8167 0.1307 0.7053 0.237 Uiso 1 1 calc R U . . .
H13C H 0.7877 0.1840 0.7145 0.237 Uiso 1 1 calc R U . . .
C14 C 0.9013(9) 0.2817(9) 0.7455(3) 0.153(5) Uani 1 1 d . . . . .
H14A H 0.8683 0.2991 0.7401 0.230 Uiso 1 1 calc R U . . .
H14B H 0.9511 0.3225 0.7458 0.230 Uiso 1 1 calc R U . . .
H14C H 0.8886 0.2596 0.7649 0.230 Uiso 1 1 calc R U . . .
C15 C 1.0217(5) 0.1401(5) 0.8257(2) 0.091(3) Uani 1 1 d . . . . .
H15A H 1.0100 0.1154 0.8449 0.110 Uiso 1 1 calc R U . . .
H15B H 1.0708 0.1504 0.8203 0.110 Uiso 1 1 calc R U . . .
C16 C 1.0231(5) 0.2102(5) 0.8291(2) 0.094(3) Uani 1 1 d . . . . .
H16A H 1.0401 0.2372 0.8105 0.113 Uiso 1 1 calc R U . . .
H16B H 1.0592 0.2389 0.8442 0.113 Uiso 1 1 calc R U . . .
C17 C 0.8709(6) 0.0900(6) 0.8752(3) 0.101(3) Uani 1 1 d . . . . .
C18 C 0.9170(6) 0.1644(6) 0.8743(2) 0.108(3) Uani 1 1 d . . . . .
C19 C 0.9425(7) 0.2065(7) 0.8992(3) 0.120(4) Uani 1 1 d . . . . .
H19 H 0.9750 0.2571 0.8976 0.144 Uiso 1 1 calc R U . . .
C20 C 0.9208(7) 0.1751(8) 0.9264(3) 0.123(4) Uani 1 1 d . . . . .
C21 C 0.8723(7) 0.1021(7) 0.9270(2) 0.116(4) Uani 1 1 d . . . . .
H21 H 0.8567 0.0800 0.9456 0.139 Uiso 1 1 calc R U . . .
C22 C 0.8441(6) 0.0576(6) 0.9025(2) 0.106(3) Uani 1 1 d . . . . .
C23 C 0.7894(7) -0.0236(7) 0.9050(3) 0.122(4) Uani 1 1 d . . . . .
C24 C 0.7235(8) -0.0434(8) 0.8852(3) 0.161(6) Uani 1 1 d . . . . .
H24A H 0.7379 -0.0406 0.8648 0.242 Uiso 1 1 calc R U . . .
H24B H 0.7060 -0.0095 0.8887 0.242 Uiso 1 1 calc R U . . .
H24C H 0.6849 -0.0928 0.8897 0.242 Uiso 1 1 calc R U . . .
C25 C 0.8249(9) -0.0669(7) 0.8956(3) 0.145(5) Uani 1 1 d . . . . .
H25A H 0.8644 -0.0574 0.9090 0.217 Uiso 1 1 calc R U . . .
H25B H 0.8443 -0.0525 0.8758 0.217 Uiso 1 1 calc R U . . .
H25C H 0.7889 -0.1186 0.8958 0.217 Uiso 1 1 calc R U . . .
C26 C 0.7629(9) -0.0434(8) 0.9363(3) 0.154(5) Uani 1 1 d . . . . .
H26A H 0.7277 -0.0953 0.9375 0.232 Uiso 1 1 calc R U . . .
H26B H 0.7399 -0.0158 0.9425 0.232 Uiso 1 1 calc R U . . .
H26C H 0.8041 -0.0320 0.9491 0.232 Uiso 1 1 calc R U . . .
C27 C 0.9499(9) 0.2183(9) 0.9560(4) 0.156(6) Uani 1 1 d . . . . .
C28A C 0.987(3) 0.193(3) 0.9733(12) 0.23(2) Uiso 0.47(2) 1 d . . P A 1
H28A H 1.0122 0.2280 0.9890 0.338 Uiso 0.47(2) 1 calc R U P A 1
H28B H 1.0224 0.1886 0.9613 0.338 Uiso 0.47(2) 1 calc R U P A 1
H28C H 0.9525 0.1462 0.9816 0.338 Uiso 0.47(2) 1 calc R U P A 1
C29A C 0.885(3) 0.225(3) 0.9681(13) 0.26(3) Uiso 0.47(2) 1 d . . P A 1
H29A H 0.9008 0.2554 0.9857 0.384 Uiso 0.47(2) 1 calc R U P A 1
H29B H 0.8452 0.1769 0.9730 0.384 Uiso 0.47(2) 1 calc R U P A 1
H29C H 0.8695 0.2474 0.9534 0.384 Uiso 0.47(2) 1 calc R U P A 1
C30A C 1.000(2) 0.305(2) 0.9482(8) 0.173(15) Uiso 0.47(2) 1 d . . P A 1
H30A H 0.9692 0.3243 0.9423 0.260 Uiso 0.47(2) 1 calc R U P A 1
H30B H 1.0332 0.3108 0.9321 0.260 Uiso 0.47(2) 1 calc R U P A 1
H30C H 1.0286 0.3309 0.9653 0.260 Uiso 0.47(2) 1 calc R U P A 1
C28B C 1.027(2) 0.2343(19) 0.9591(8) 0.172(13) Uiso 0.53(2) 1 d . . P A 2
H28D H 1.0547 0.2787 0.9705 0.258 Uiso 0.53(2) 1 calc R U P A 2
H28E H 1.0487 0.2406 0.9398 0.258 Uiso 0.53(2) 1 calc R U P A 2
H28F H 1.0273 0.1939 0.9691 0.258 Uiso 0.53(2) 1 calc R U P A 2
C29B C 0.9098(17) 0.1792(17) 0.9805(6) 0.153(11) Uiso 0.53(2) 1 d . . P A 2
H29D H 0.9300 0.2089 0.9980 0.229 Uiso 0.53(2) 1 calc R U P A 2
H29E H 0.9123 0.1348 0.9824 0.229 Uiso 0.53(2) 1 calc R U P A 2
H29F H 0.8592 0.1668 0.9782 0.229 Uiso 0.53(2) 1 calc R U P A 2
C30B C 0.942(2) 0.284(2) 0.9509(7) 0.172(13) Uiso 0.53(2) 1 d . . P A 2
H30D H 0.8908 0.2705 0.9529 0.258 Uiso 0.53(2) 1 calc R U P A 2
H30E H 0.9587 0.3031 0.9313 0.258 Uiso 0.53(2) 1 calc R U P A 2
H30F H 0.9707 0.3215 0.9653 0.258 Uiso 0.53(2) 1 calc R U P A 2
C31 C 0.7196(8) -0.0413(9) 0.7956(3) 0.133(5) Uani 1 1 d . . . . .
H31 H 0.6947 -0.0189 0.8037 0.160 Uiso 1 1 calc R U . . .
C32 C 0.7811(6) 0.1187(8) 0.8217(2) 0.118(4) Uani 1 1 d . . . . .
C33A C 0.723(2) 0.131(2) 0.8277(8) 0.133(12) Uiso 0.47(2) 1 d . . P A 1
H33A H 0.6761 0.0851 0.8292 0.159 Uiso 0.47(2) 1 calc R U P A 1
H33B H 0.7192 0.1631 0.8132 0.159 Uiso 0.47(2) 1 calc R U P A 1
C34A C 0.756(3) 0.177(3) 0.8644(11) 0.23(2) Uiso 0.47(2) 1 d . . P A 1
H34A H 0.8085 0.1998 0.8654 0.347 Uiso 0.47(2) 1 calc R U P A 1
H34B H 0.7341 0.1403 0.8799 0.347 Uiso 0.47(2) 1 calc R U P A 1
H34C H 0.7411 0.2131 0.8669 0.347 Uiso 0.47(2) 1 calc R U P A 1
C33B C 0.740(2) 0.164(2) 0.8294(7) 0.144(12) Uiso 0.53(2) 1 d . . P A 2
H33C H 0.7744 0.2159 0.8333 0.172 Uiso 0.53(2) 1 calc R U P A 2
H33D H 0.7056 0.1598 0.8139 0.172 Uiso 0.53(2) 1 calc R U P A 2
C34B C 0.708(3) 0.131(3) 0.8520(11) 0.215(18) Uiso 0.53(2) 1 d . . P A 2
H34D H 0.6606 0.1290 0.8532 0.323 Uiso 0.53(2) 1 calc R U P A 2
H34E H 0.7368 0.1570 0.8691 0.323 Uiso 0.53(2) 1 calc R U P A 2
H34F H 0.7002 0.0821 0.8515 0.323 Uiso 0.53(2) 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
W1 C32 1.726(11) . ?
W1 O1 1.957(7) . ?
W1 O3 1.959(9) . ?
W1 O2 1.992(6) . ?
W1 S2 2.545(3) . ?
W1 S1 2.684(3) . ?
S1 C2 1.769(9) . ?
S1 C15 1.819(9) . ?
S2 C18 1.792(12) . ?
S2 C16 1.813(11) . ?
O1 C1 1.348(12) . ?
O2 C17 1.330(12) . ?
O3 C31 1.230(15) . ?
O4 C31 1.212(16) . ?
C1 C2 1.407(14) . ?
C1 C6 1.437(14) . ?
C2 C3 1.372(14) . ?
C3 C4 1.386(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.406(15) . ?
C4 C7 1.532(16) . ?
C5 C6 1.388(16) . ?
C5 H5 0.9500 . ?
C6 C11 1.550(16) . ?
C7 C8B 1.48(4) . ?
C7 C9A 1.50(4) . ?
C7 C9B 1.51(3) . ?
C7 C8A 1.51(2) . ?
C7 C10 1.55(2) . ?
C8A H8A 0.9800 . ?
C8A H8B 0.9800 . ?
C8A H8C 0.9800 . ?
C9A C10 2.03(5) . ?
C9A H9A 0.9800 . ?
C9A H9B 0.9800 . ?
C9A H9C 0.9800 . ?
C8B C10 1.97(5) . ?
C8B H8D 0.9800 . ?
C8B H8E 0.9800 . ?
C8B H8F 0.9800 . ?
C9B H9D 0.9800 . ?
C9B H9E 0.9800 . ?
C9B H9F 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C10 H10D 0.9800 . ?
C10 H10E 0.9800 . ?
C10 H10F 0.9800 . ?
C11 C13 1.498(19) . ?
C11 C14 1.534(19) . ?
C11 C12 1.580(17) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.488(13) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.388(14) . ?
C17 C22 1.408(15) . ?
C18 C19 1.386(16) . ?
C19 C20 1.382(17) . ?
C19 H19 0.9500 . ?
C20 C21 1.373(17) . ?
C20 C27 1.583(19) . ?
C21 C22 1.399(15) . ?
C21 H21 0.9500 . ?
C22 C23 1.534(16) . ?
C23 C25 1.522(18) . ?
C23 C26 1.522(16) . ?
C23 C24 1.544(19) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28A 1.40(5) . ?
C27 C29B 1.41(3) . ?
C27 C28B 1.51(4) . ?
C27 C30B 1.52(4) . ?
C27 C29A 1.56(6) . ?
C27 C30A 1.64(4) . ?
C28A H28A 0.9800 . ?
C28A H28B 0.9800 . ?
C28A H28C 0.9800 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C28B H28D 0.9800 . ?
C28B H28E 0.9800 . ?
C28B H28F 0.9800 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31 H31 0.9500 . ?
C32 C33A 1.42(4) . ?
C32 C33B 1.64(4) . ?
C33A C34A 1.89(6) . ?
C33A H33A 0.9900 . ?
C33A H33B 0.9900 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C33B C34B 1.25(5) . ?
C33B H33C 0.9900 . ?
C33B H33D 0.9900 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 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
C32 W1 O1 97.5(4) . . ?
C32 W1 O3 106.5(5) . . ?
O1 W1 O3 101.0(3) . . ?
C32 W1 O2 100.5(4) . . ?
O1 W1 O2 154.2(3) . . ?
O3 W1 O2 91.5(3) . . ?
C32 W1 S2 87.2(5) . . ?
O1 W1 S2 85.9(2) . . ?
O3 W1 S2 163.6(2) . . ?
O2 W1 S2 76.7(2) . . ?
C32 W1 S1 168.5(5) . . ?
O1 W1 S1 77.3(2) . . ?
O3 W1 S1 84.7(2) . . ?
O2 W1 S1 81.61(19) . . ?
S2 W1 S1 82.28(8) . . ?
C2 S1 C15 104.3(5) . . ?
C2 S1 W1 95.2(4) . . ?
C15 S1 W1 99.5(3) . . ?
C18 S2 C16 105.0(5) . . ?
C18 S2 W1 95.5(4) . . ?
C16 S2 W1 104.6(3) . . ?
C1 O1 W1 128.3(6) . . ?
C17 O2 W1 124.5(7) . . ?
C31 O3 W1 124.6(10) . . ?
O1 C1 C2 122.7(9) . . ?
O1 C1 C6 118.9(10) . . ?
C2 C1 C6 118.3(10) . . ?
C3 C2 C1 123.0(9) . . ?
C3 C2 S1 120.5(8) . . ?
C1 C2 S1 116.1(8) . . ?
C2 C3 C4 120.2(10) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 116.9(10) . . ?
C3 C4 C7 121.9(11) . . ?
C5 C4 C7 121.2(10) . . ?
C6 C5 C4 125.4(10) . . ?
C6 C5 H5 117.3 . . ?
C4 C5 H5 117.3 . . ?
C5 C6 C1 116.0(10) . . ?
C5 C6 C11 124.2(10) . . ?
C1 C6 C11 119.7(11) . . ?
C8B C7 C9B 135(2) . . ?
C9A C7 C8A 121(2) . . ?
C8B C7 C4 105(2) . . ?
C9A C7 C4 110(2) . . ?
C9B C7 C4 108.9(13) . . ?
C8A C7 C4 114.5(11) . . ?
C8B C7 C10 81(2) . . ?
C9A C7 C10 84(2) . . ?
C9B C7 C10 113.9(16) . . ?
C8A C7 C10 115.4(13) . . ?
C4 C7 C10 108.1(13) . . ?
C7 C8A H8A 109.5 . . ?
C7 C8A H8B 109.5 . . ?
H8A C8A H8B 109.5 . . ?
C7 C8A H8C 109.5 . . ?
H8A C8A H8C 109.5 . . ?
H8B C8A H8C 109.5 . . ?
C7 C9A C10 49.3(15) . . ?
C7 C9A H9A 109.5 . . ?
C10 C9A H9A 75.0 . . ?
C7 C9A H9B 109.5 . . ?
C10 C9A H9B 156.5 . . ?
H9A C9A H9B 109.5 . . ?
C7 C9A H9C 109.5 . . ?
C10 C9A H9C 89.7 . . ?
H9A C9A H9C 109.5 . . ?
H9B C9A H9C 109.5 . . ?
C7 C8B C10 51.0(16) . . ?
C7 C8B H8D 109.5 . . ?
C10 C8B H8D 140.4 . . ?
C7 C8B H8E 109.5 . . ?
C10 C8B H8E 61.4 . . ?
H8D C8B H8E 109.5 . . ?
C7 C8B H8F 109.5 . . ?
C10 C8B H8F 109.7 . . ?
H8D C8B H8F 109.5 . . ?
H8E C8B H8F 109.5 . . ?
C7 C9B H9D 109.5 . . ?
C7 C9B H9E 109.5 . . ?
H9D C9B H9E 109.5 . . ?
C7 C9B H9F 109.5 . . ?
H9D C9B H9F 109.5 . . ?
H9E C9B H9F 109.5 . . ?
C7 C10 C8B 47.9(15) . . ?
C7 C10 C9A 47.2(14) . . ?
C7 C10 H10A 109.5 . . ?
C9A C10 H10A 124.6 . . ?
C7 C10 H10B 109.5 . . ?
C9A C10 H10B 125.2 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
C9A C10 H10C 62.3 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C10 H10D 109.5 . . ?
C8B C10 H10D 101.0 . . ?
C7 C10 H10E 109.5 . . ?
C8B C10 H10E 147.7 . . ?
H10D C10 H10E 109.5 . . ?
C7 C10 H10F 109.5 . . ?
C8B C10 H10F 68.6 . . ?
H10D C10 H10F 109.5 . . ?
H10E C10 H10F 109.5 . . ?
C13 C11 C14 111.7(13) . . ?
C13 C11 C6 109.6(12) . . ?
C14 C11 C6 110.5(11) . . ?
C13 C11 C12 109.1(11) . . ?
C14 C11 C12 107.1(12) . . ?
C6 C11 C12 108.8(11) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 S1 115.3(7) . . ?
C16 C15 H15A 108.4 . . ?
S1 C15 H15A 108.4 . . ?
C16 C15 H15B 108.4 . . ?
S1 C15 H15B 108.4 . . ?
H15A C15 H15B 107.5 . . ?
C15 C16 S2 116.0(7) . . ?
C15 C16 H16A 108.3 . . ?
S2 C16 H16A 108.3 . . ?
C15 C16 H16B 108.3 . . ?
S2 C16 H16B 108.3 . . ?
H16A C16 H16B 107.4 . . ?
O2 C17 C18 118.6(10) . . ?
O2 C17 C22 123.3(9) . . ?
C18 C17 C22 118.1(10) . . ?
C19 C18 C17 122.7(11) . . ?
C19 C18 S2 121.4(9) . . ?
C17 C18 S2 115.8(9) . . ?
C20 C19 C18 120.2(12) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 C19 116.7(11) . . ?
C21 C20 C27 119.7(12) . . ?
C19 C20 C27 123.6(13) . . ?
C20 C21 C22 125.2(11) . . ?
C20 C21 H21 117.4 . . ?
C22 C21 H21 117.4 . . ?
C21 C22 C17 116.8(11) . . ?
C21 C22 C23 122.1(10) . . ?
C17 C22 C23 121.0(9) . . ?
C25 C23 C26 109.1(12) . . ?
C25 C23 C22 109.5(11) . . ?
C26 C23 C22 110.6(10) . . ?
C25 C23 C24 109.1(12) . . ?
C26 C23 C24 108.6(12) . . ?
C22 C23 C24 109.9(11) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29B C27 C28B 109(2) . . ?
C29B C27 C30B 111(2) . . ?
C28B C27 C30B 115(2) . . ?
C28A C27 C29A 122(3) . . ?
C28A C27 C20 113(3) . . ?
C29B C27 C20 113.3(17) . . ?
C28B C27 C20 106.2(16) . . ?
C30B C27 C20 102.4(19) . . ?
C29A C27 C20 105(2) . . ?
C28A C27 C30A 112(3) . . ?
C29A C27 C30A 95(3) . . ?
C20 C27 C30A 108.2(18) . . ?
C27 C28A H28A 109.5 . . ?
C27 C28A H28B 109.5 . . ?
H28A C28A H28B 109.5 . . ?
C27 C28A H28C 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C27 C29A H29A 109.5 . . ?
C27 C29A H29B 109.5 . . ?
H29A C29A H29B 109.5 . . ?
C27 C29A H29C 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C27 C30A H30A 109.5 . . ?
C27 C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C27 C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C27 C28B H28D 109.5 . . ?
C27 C28B H28E 109.5 . . ?
H28D C28B H28E 109.5 . . ?
C27 C28B H28F 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C27 C29B H29D 109.5 . . ?
C27 C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C27 C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C27 C30B H30D 109.5 . . ?
C27 C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C27 C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
O4 C31 O3 126.9(16) . . ?
O4 C31 H31 116.5 . . ?
O3 C31 H31 116.5 . . ?
C33A C32 W1 172(2) . . ?
C33B C32 W1 166.0(17) . . ?
C32 C33A C34A 98(3) . . ?
C32 C33A H33A 112.2 . . ?
C34A C33A H33A 112.2 . . ?
C32 C33A H33B 112.2 . . ?
C34A C33A H33B 112.2 . . ?
H33A C33A H33B 109.8 . . ?
C33A C34A H34A 109.5 . . ?
C33A C34A H34B 109.5 . . ?
H34A C34A H34B 109.5 . . ?
C33A C34A H34C 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C34B C33B C32 99(3) . . ?
C34B C33B H33C 112.0 . . ?
C32 C33B H33C 112.0 . . ?
C34B C33B H33D 112.0 . . ?
C32 C33B H33D 112.0 . . ?
H33C C33B H33D 109.7 . . ?
C33B C34B H34D 109.5 . . ?
C33B C34B H34E 109.5 . . ?
H34D C34B H34E 109.5 . . ?
C33B C34B H34F 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W1 O1 C1 C2 -9.2(15) . . . . ?
W1 O1 C1 C6 172.5(8) . . . . ?
O1 C1 C2 C3 179.2(10) . . . . ?
C6 C1 C2 C3 -2.5(17) . . . . ?
O1 C1 C2 S1 6.2(14) . . . . ?
C6 C1 C2 S1 -175.6(8) . . . . ?
C15 S1 C2 C3 84.0(10) . . . . ?
W1 S1 C2 C3 -174.8(9) . . . . ?
C15 S1 C2 C1 -102.7(9) . . . . ?
W1 S1 C2 C1 -1.6(8) . . . . ?
C1 C2 C3 C4 2.5(17) . . . . ?
S1 C2 C3 C4 175.3(9) . . . . ?
C2 C3 C4 C5 -0.6(17) . . . . ?
C2 C3 C4 C7 179.5(11) . . . . ?
C3 C4 C5 C6 -1.3(19) . . . . ?
C7 C4 C5 C6 178.6(12) . . . . ?
C4 C5 C6 C1 1.3(19) . . . . ?
C4 C5 C6 C11 -179.0(12) . . . . ?
O1 C1 C6 C5 178.9(10) . . . . ?
C2 C1 C6 C5 0.6(16) . . . . ?
O1 C1 C6 C11 -0.8(17) . . . . ?
C2 C1 C6 C11 -179.1(11) . . . . ?
C3 C4 C7 C8B 39(3) . . . . ?
C5 C4 C7 C8B -141(2) . . . . ?
C3 C4 C7 C9A -146(2) . . . . ?
C5 C4 C7 C9A 34(3) . . . . ?
C3 C4 C7 C9B -111.4(18) . . . . ?
C5 C4 C7 C9B 69(2) . . . . ?
C3 C4 C7 C8A -6(2) . . . . ?
C5 C4 C7 C8A 174.4(14) . . . . ?
C3 C4 C7 C10 124.4(14) . . . . ?
C5 C4 C7 C10 -55.5(16) . . . . ?
C8B C7 C9A C10 65(5) . . . . ?
C9B C7 C9A C10 158(4) . . . . ?
C8A C7 C9A C10 115.9(18) . . . . ?
C4 C7 C9A C10 -107.0(16) . . . . ?
C9A C7 C8B C10 -65(5) . . . . ?
C9B C7 C8B C10 -115(3) . . . . ?
C8A C7 C8B C10 -144(3) . . . . ?
C4 C7 C8B C10 106.5(15) . . . . ?
C9A C7 C10 C8B 148(3) . . . . ?
C9B C7 C10 C8B 136(3) . . . . ?
C8A C7 C10 C8B 26(2) . . . . ?
C4 C7 C10 C8B -103(2) . . . . ?
C8B C7 C10 C9A -148(3) . . . . ?
C9B C7 C10 C9A -13(3) . . . . ?
C8A C7 C10 C9A -122(2) . . . . ?
C4 C7 C10 C9A 109(2) . . . . ?
C5 C6 C11 C13 118.3(14) . . . . ?
C1 C6 C11 C13 -62.0(16) . . . . ?
C5 C6 C11 C14 -118.1(14) . . . . ?
C1 C6 C11 C14 61.6(16) . . . . ?
C5 C6 C11 C12 -0.9(19) . . . . ?
C1 C6 C11 C12 178.8(12) . . . . ?
C2 S1 C15 C16 53.9(8) . . . . ?
W1 S1 C15 C16 -44.0(7) . . . . ?
S1 C15 C16 S2 57.5(9) . . . . ?
C18 S2 C16 C15 64.7(8) . . . . ?
W1 S2 C16 C15 -35.2(8) . . . . ?
W1 O2 C17 C18 -32.8(13) . . . . ?
W1 O2 C17 C22 145.9(9) . . . . ?
O2 C17 C18 C19 -175.3(10) . . . . ?
C22 C17 C18 C19 6.0(18) . . . . ?
O2 C17 C18 S2 8.1(14) . . . . ?
C22 C17 C18 S2 -170.6(9) . . . . ?
C16 S2 C18 C19 87.6(10) . . . . ?
W1 S2 C18 C19 -165.7(9) . . . . ?
C16 S2 C18 C17 -95.7(9) . . . . ?
W1 S2 C18 C17 11.0(9) . . . . ?
C17 C18 C19 C20 -1.7(19) . . . . ?
S2 C18 C19 C20 174.7(10) . . . . ?
C18 C19 C20 C21 -1.6(19) . . . . ?
C18 C19 C20 C27 177.1(13) . . . . ?
C19 C20 C21 C22 1(2) . . . . ?
C27 C20 C21 C22 -178.2(13) . . . . ?
C20 C21 C22 C17 4(2) . . . . ?
C20 C21 C22 C23 -179.2(13) . . . . ?
O2 C17 C22 C21 174.6(11) . . . . ?
C18 C17 C22 C21 -6.7(17) . . . . ?
O2 C17 C22 C23 -2.5(18) . . . . ?
C18 C17 C22 C23 176.2(11) . . . . ?
C21 C22 C23 C25 -111.1(13) . . . . ?
C17 C22 C23 C25 65.8(15) . . . . ?
C21 C22 C23 C26 9.2(19) . . . . ?
C17 C22 C23 C26 -173.8(12) . . . . ?
C21 C22 C23 C24 129.1(13) . . . . ?
C17 C22 C23 C24 -53.9(16) . . . . ?
C21 C20 C27 C28A 61(3) . . . . ?
C19 C20 C27 C28A -118(3) . . . . ?
C21 C20 C27 C29B -14(3) . . . . ?
C19 C20 C27 C29B 168(2) . . . . ?
C21 C20 C27 C28B 106(2) . . . . ?
C19 C20 C27 C28B -72(2) . . . . ?
C21 C20 C27 C30B -133(2) . . . . ?
C19 C20 C27 C30B 48(2) . . . . ?
C21 C20 C27 C29A -74(3) . . . . ?
C19 C20 C27 C29A 107(3) . . . . ?
C21 C20 C27 C30A -175(2) . . . . ?
C19 C20 C27 C30A 7(3) . . . . ?
W1 O3 C31 O4 179.7(13) . . . . ?
O1 W1 C32 C33B -51(6) . . . . ?
O3 W1 C32 C33B -155(6) . . . . ?
O2 W1 C32 C33B 111(6) . . . . ?
S2 W1 C32 C33B 35(6) . . . . ?
S1 W1 C32 C33B 11(7) . . . . ?
C33B C32 C33A C34A -57(5) . . . . ?
C33A C32 C33B C34B 57(5) . . . . ?
W1 C32 C33B C34B -134(5) . . . . ?

_refine_diff_density_max         0.544
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.090

_shelxl_version_number           2013-4


# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 234 41 ' '
2 0.000 0.000 0.500 719 146 ' '
3 0.333 0.667 0.167 716 146 ' '
4 0.333 0.667 0.667 237 41 ' '
5 0.667 0.333 0.833 717 146 ' '
6 0.667 0.333 0.333 237 41 ' '
_platon_squeeze_void_probe_radius 1.20
#==END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: thf and n-hexane'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
