# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 
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data_lcza110517
_database_code_depnum_ccdc_archive 'CCDC 1476805'
_audit_update_record             
;
2016-08-02 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H30 Cl2 O4'
_chemical_formula_sum            'C32 H30 Cl2 O4'
_chemical_formula_weight         549.46

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

_space_group_crystal_system      trigonal
_space_group_IT_number           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                   36.04(3)
_cell_length_b                   36.04(3)
_cell_length_c                   11.643(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     13095(21)
_cell_formula_units_Z            18
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9693
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      24.94

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_F_000             5184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.257
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49636
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.867
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             6561
_reflns_number_gt                4087
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_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)+(0.1810P)²] 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         6561
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0798
_refine_ls_wR_factor_ref         0.2728
_refine_ls_wR_factor_gt          0.2445
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
C1 C 0.81129(8) 0.72809(9) 0.2015(3) 0.0415(6) Uani 1 1 d . . . . .
C2 C 0.78560(9) 0.68429(10) 0.1781(3) 0.0481(7) Uani 1 1 d . . . . .
H2 H 0.7633 0.6667 0.2298 0.058 Uiso 1 1 calc R U . . .
C3 C 0.79203(10) 0.66642(10) 0.0824(3) 0.0517(8) Uani 1 1 d . . . . .
H3 H 0.7736 0.6369 0.0666 0.062 Uiso 1 1 calc R U . . .
C4 C 0.82580(10) 0.69153(10) 0.0072(3) 0.0487(7) Uani 1 1 d . . . . .
H4 H 0.8306 0.6787 -0.0581 0.058 Uiso 1 1 calc R U . . .
C5 C 0.85251(9) 0.73550(9) 0.0280(2) 0.0400(6) Uani 1 1 d . . . . .
C6 C 0.84319(8) 0.75259(8) 0.1239(2) 0.0374(6) Uani 1 1 d . . . . .
C7 C 0.85319(11) 0.82283(10) 0.0980(3) 0.0558(8) Uani 1 1 d . . . . .
H7A H 0.8241 0.8137 0.1276 0.067 Uiso 1 1 calc R U . . .
H7B H 0.8516 0.8200 0.0133 0.067 Uiso 1 1 calc R U . . .
C8 C 0.88316(17) 0.86789(13) 0.1311(4) 0.0846(13) Uani 1 1 d . . . . .
H8A H 0.8748 0.8868 0.0908 0.102 Uiso 1 1 calc R U . . .
H8B H 0.9124 0.8758 0.1052 0.102 Uiso 1 1 calc R U . . .
C9 C 0.89066(9) 0.76233(10) -0.0497(3) 0.0440(6) Uani 1 1 d . . . . .
H9A H 0.8811 0.7564 -0.1307 0.053 Uiso 1 1 calc R U . . .
H9B H 0.9010 0.7930 -0.0349 0.053 Uiso 1 1 calc R U . . .
C10 C 0.92763(9) 0.75382(9) -0.0329(2) 0.0396(6) Uani 1 1 d . . . . .
C11 C 0.93599(10) 0.72998(10) -0.1112(3) 0.0494(7) Uani 1 1 d . . . . .
H11 H 0.9175 0.7175 -0.1753 0.059 Uiso 1 1 calc R U . . .
C12 C 0.97068(11) 0.72402(12) -0.0976(3) 0.0591(9) Uani 1 1 d . . . . .
H12 H 0.9765 0.7084 -0.1534 0.071 Uiso 1 1 calc R U . . .
C13 C 0.99698(10) 0.74088(11) -0.0024(3) 0.0506(7) Uani 1 1 d . . . . .
H13 H 1.0206 0.7364 0.0068 0.061 Uiso 1 1 calc R U . . .
C14 C 0.98935(8) 0.76420(9) 0.0795(3) 0.0421(6) Uani 1 1 d . . . . .
C15 C 0.95502(8) 0.77154(8) 0.0614(2) 0.0389(6) Uani 1 1 d . . . . .
C16 C 1.01913(9) 0.78269(11) 0.1820(3) 0.0486(7) Uani 1 1 d . . . . .
H16A H 1.0442 0.7788 0.1699 0.058 Uiso 1 1 calc R U . . .
H16B H 1.0298 0.8139 0.1858 0.058 Uiso 1 1 calc R U . . .
C17 C 0.99860(8) 0.76274(9) 0.2955(3) 0.0435(7) Uani 1 1 d . . . . .
C18 C 0.99434(10) 0.72358(10) 0.3285(3) 0.0498(7) Uani 1 1 d . . . . .
H18 H 1.0050 0.7099 0.2799 0.060 Uiso 1 1 calc R U . . .
C19 C 0.97482(11) 0.70450(10) 0.4307(3) 0.0538(8) Uani 1 1 d . . . . .
H19 H 0.9736 0.6786 0.4538 0.065 Uiso 1 1 calc R U . . .
C20 C 0.95719(10) 0.72252(10) 0.4993(3) 0.0520(8) Uani 1 1 d . . . . .
H20 H 0.9429 0.7083 0.5680 0.062 Uiso 1 1 calc R U . . .
C21 C 0.95983(9) 0.76131(9) 0.4704(3) 0.0423(6) Uani 1 1 d . . . . .
C22 C 0.98249(8) 0.78159(8) 0.3701(3) 0.0410(6) Uani 1 1 d . . . . .
C23 C 1.02515(11) 0.85734(11) 0.3866(4) 0.0667(10) Uani 1 1 d . . . . .
H23A H 1.0511 0.8570 0.3607 0.080 Uiso 1 1 calc R U . . .
H23B H 1.0242 0.8560 0.4716 0.080 Uiso 1 1 calc R U . . .
C24 C 1.02674(18) 0.89667(13) 0.3478(5) 0.0968(16) Uani 1 1 d . . . . .
H24A H 1.0515 0.9215 0.3842 0.116 Uiso 1 1 calc R U . . .
H24B H 1.0004 0.8964 0.3736 0.116 Uiso 1 1 calc R U . . .
C25 C 0.93758(10) 0.77927(11) 0.5438(3) 0.0507(7) Uani 1 1 d . . . . .
H25A H 0.9445 0.7781 0.6255 0.061 Uiso 1 1 calc R U . . .
H25B H 0.9489 0.8097 0.5233 0.061 Uiso 1 1 calc R U . . .
C26 C 0.88926(10) 0.75520(9) 0.5292(2) 0.0433(7) Uani 1 1 d . . . . .
C27 C 0.86187(11) 0.72677(11) 0.6134(3) 0.0536(8) Uani 1 1 d . . . . .
H27 H 0.8738 0.7213 0.6796 0.064 Uiso 1 1 calc R U . . .
C28 C 0.81807(11) 0.70668(11) 0.6015(3) 0.0560(8) Uani 1 1 d . . . . .
H28 H 0.8000 0.6883 0.6605 0.067 Uiso 1 1 calc R U . . .
C29 C 0.80030(10) 0.71309(10) 0.5042(3) 0.0494(7) Uani 1 1 d . . . . .
H29 H 0.7700 0.6986 0.4966 0.059 Uiso 1 1 calc R U . . .
C30 C 0.82572(9) 0.74042(9) 0.4166(2) 0.0415(6) Uani 1 1 d . . . . .
C31 C 0.87067(9) 0.76193(9) 0.4318(2) 0.0417(6) Uani 1 1 d . . . . .
C32 C 0.80480(9) 0.74723(10) 0.3122(3) 0.0483(7) Uani 1 1 d . . . . .
H32A H 0.8166 0.7784 0.3009 0.058 Uiso 1 1 calc R U . . .
H32B H 0.7737 0.7342 0.3268 0.058 Uiso 1 1 calc R U . . .
O1 O 0.86889(6) 0.79685(6) 0.14624(18) 0.0420(5) Uani 1 1 d . . . . .
O2 O 0.94690(7) 0.79696(8) 0.1309(2) 0.0553(6) Uani 1 1 d . . . . .
H2A H 0.9668 0.8091 0.1790 0.083 Uiso 1 1 calc R U . . .
O3 O 0.98765(6) 0.82122(6) 0.33992(19) 0.0469(5) Uani 1 1 d . . . . .
O4 O 0.89847(6) 0.79108(8) 0.3556(2) 0.0596(6) Uani 1 1 d . . . . .
H4A H 0.8847 0.7940 0.3015 0.089 Uiso 1 1 calc R U . . .
Cl1 Cl 0.88428(8) 0.87705(5) 0.28047(16) 0.1452(8) Uani 1 1 d . . . . .
Cl2 Cl 1.03120(8) 0.90322(5) 0.19563(17) 0.1586(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.379(4) . ?
C1 C2 1.401(4) . ?
C1 C32 1.533(4) . ?
C2 C3 1.364(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.401(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(4) . ?
C5 C9 1.522(4) . ?
C6 O1 1.411(3) . ?
C7 O1 1.429(3) . ?
C7 C8 1.483(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 Cl1 1.767(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.522(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.385(4) . ?
C10 C15 1.399(4) . ?
C11 C12 1.379(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.386(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(4) . ?
C14 C16 1.518(4) . ?
C15 O2 1.359(3) . ?
C16 C17 1.510(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.395(4) . ?
C17 C22 1.396(4) . ?
C18 C19 1.378(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.394(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.403(4) . ?
C21 C25 1.520(4) . ?
C22 O3 1.390(3) . ?
C23 O3 1.435(4) . ?
C23 C24 1.461(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 Cl2 1.784(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.518(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.399(4) . ?
C26 C27 1.405(5) . ?
C27 C28 1.375(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.376(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.396(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.414(4) . ?
C30 C32 1.514(4) . ?
C31 O4 1.357(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
O2 H2A 0.8400 . ?
O4 H4A 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 C1 C2 117.6(3) . . ?
C6 C1 C32 121.9(3) . . ?
C2 C1 C32 120.5(3) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 120.3(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 117.1(3) . . ?
C6 C5 C9 122.4(2) . . ?
C4 C5 C9 120.4(3) . . ?
C1 C6 C5 123.3(3) . . ?
C1 C6 O1 117.9(2) . . ?
C5 C6 O1 118.7(2) . . ?
O1 C7 C8 107.8(3) . . ?
O1 C7 H7A 110.2 . . ?
C8 C7 H7A 110.2 . . ?
O1 C7 H7B 110.2 . . ?
C8 C7 H7B 110.2 . . ?
H7A C7 H7B 108.5 . . ?
C7 C8 Cl1 113.4(3) . . ?
C7 C8 H8A 108.9 . . ?
Cl1 C8 H8A 108.9 . . ?
C7 C8 H8B 108.9 . . ?
Cl1 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C5 113.5(2) . . ?
C10 C9 H9A 108.9 . . ?
C5 C9 H9A 108.9 . . ?
C10 C9 H9B 108.9 . . ?
C5 C9 H9B 108.9 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C15 118.5(3) . . ?
C11 C10 C9 121.6(3) . . ?
C15 C10 C9 119.9(2) . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 119.9(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.1(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C15 118.1(3) . . ?
C13 C14 C16 119.7(3) . . ?
C15 C14 C16 122.1(3) . . ?
O2 C15 C10 115.8(2) . . ?
O2 C15 C14 123.0(3) . . ?
C10 C15 C14 121.3(3) . . ?
C17 C16 C14 114.1(2) . . ?
C17 C16 H16A 108.7 . . ?
C14 C16 H16A 108.7 . . ?
C17 C16 H16B 108.7 . . ?
C14 C16 H16B 108.7 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C22 117.3(3) . . ?
C18 C17 C16 120.2(3) . . ?
C22 C17 C16 122.5(3) . . ?
C19 C18 C17 120.9(3) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C18 120.6(3) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
C19 C20 C21 121.3(3) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C20 C21 C22 117.0(3) . . ?
C20 C21 C25 120.4(3) . . ?
C22 C21 C25 122.6(3) . . ?
O3 C22 C17 117.9(3) . . ?
O3 C22 C21 119.3(3) . . ?
C17 C22 C21 122.7(3) . . ?
O3 C23 C24 109.0(3) . . ?
O3 C23 H23A 109.9 . . ?
C24 C23 H23A 109.9 . . ?
O3 C23 H23B 109.9 . . ?
C24 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C23 C24 Cl2 113.1(4) . . ?
C23 C24 H24A 109.0 . . ?
Cl2 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
Cl2 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C26 C25 C21 113.1(2) . . ?
C26 C25 H25A 109.0 . . ?
C21 C25 H25A 109.0 . . ?
C26 C25 H25B 109.0 . . ?
C21 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
C31 C26 C27 118.0(3) . . ?
C31 C26 C25 120.2(3) . . ?
C27 C26 C25 121.7(3) . . ?
C28 C27 C26 121.1(3) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 120.2(3) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 121.6(3) . . ?
C28 C29 H29 119.2 . . ?
C30 C29 H29 119.2 . . ?
C29 C30 C31 117.6(3) . . ?
C29 C30 C32 119.8(3) . . ?
C31 C30 C32 122.5(3) . . ?
O4 C31 C26 115.6(3) . . ?
O4 C31 C30 122.9(3) . . ?
C26 C31 C30 121.5(3) . . ?
C30 C32 C1 113.7(2) . . ?
C30 C32 H32A 108.8 . . ?
C1 C32 H32A 108.8 . . ?
C30 C32 H32B 108.8 . . ?
C1 C32 H32B 108.8 . . ?
H32A C32 H32B 107.7 . . ?
C6 O1 C7 114.6(2) . . ?
C15 O2 H2A 109.5 . . ?
C22 O3 C23 114.7(2) . . ?
C31 O4 H4A 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
C6 C1 C2 C3 0.4(4) . . . . ?
C32 C1 C2 C3 -177.4(3) . . . . ?
C1 C2 C3 C4 2.4(4) . . . . ?
C2 C3 C4 C5 -1.8(4) . . . . ?
C3 C4 C5 C6 -1.4(4) . . . . ?
C3 C4 C5 C9 176.6(3) . . . . ?
C2 C1 C6 C5 -3.9(4) . . . . ?
C32 C1 C6 C5 173.9(2) . . . . ?
C2 C1 C6 O1 179.2(2) . . . . ?
C32 C1 C6 O1 -3.0(4) . . . . ?
C4 C5 C6 C1 4.3(4) . . . . ?
C9 C5 C6 C1 -173.7(2) . . . . ?
C4 C5 C6 O1 -178.8(2) . . . . ?
C9 C5 C6 O1 3.2(4) . . . . ?
O1 C7 C8 Cl1 -65.3(4) . . . . ?
C6 C5 C9 C10 105.0(3) . . . . ?
C4 C5 C9 C10 -72.9(3) . . . . ?
C5 C9 C10 C11 104.5(3) . . . . ?
C5 C9 C10 C15 -77.8(3) . . . . ?
C15 C10 C11 C12 -0.6(4) . . . . ?
C9 C10 C11 C12 177.2(3) . . . . ?
C10 C11 C12 C13 2.1(5) . . . . ?
C11 C12 C13 C14 -0.7(5) . . . . ?
C12 C13 C14 C15 -2.1(4) . . . . ?
C12 C13 C14 C16 -179.2(3) . . . . ?
C11 C10 C15 O2 175.7(3) . . . . ?
C9 C10 C15 O2 -2.0(4) . . . . ?
C11 C10 C15 C14 -2.4(4) . . . . ?
C9 C10 C15 C14 179.8(3) . . . . ?
C13 C14 C15 O2 -174.3(3) . . . . ?
C16 C14 C15 O2 2.7(4) . . . . ?
C13 C14 C15 C10 3.7(4) . . . . ?
C16 C14 C15 C10 -179.3(3) . . . . ?
C13 C14 C16 C17 -113.0(3) . . . . ?
C15 C14 C16 C17 70.0(4) . . . . ?
C14 C16 C17 C18 80.6(3) . . . . ?
C14 C16 C17 C22 -98.1(3) . . . . ?
C22 C17 C18 C19 0.2(4) . . . . ?
C16 C17 C18 C19 -178.6(3) . . . . ?
C17 C18 C19 C20 3.4(5) . . . . ?
C18 C19 C20 C21 -2.5(5) . . . . ?
C19 C20 C21 C22 -2.0(4) . . . . ?
C19 C20 C21 C25 176.1(3) . . . . ?
C18 C17 C22 O3 178.1(2) . . . . ?
C16 C17 C22 O3 -3.1(4) . . . . ?
C18 C17 C22 C21 -4.9(4) . . . . ?
C16 C17 C22 C21 173.8(2) . . . . ?
C20 C21 C22 O3 -177.3(2) . . . . ?
C25 C21 C22 O3 4.7(4) . . . . ?
C20 C21 C22 C17 5.8(4) . . . . ?
C25 C21 C22 C17 -172.2(3) . . . . ?
O3 C23 C24 Cl2 -62.4(5) . . . . ?
C20 C21 C25 C26 -73.3(4) . . . . ?
C22 C21 C25 C26 104.6(3) . . . . ?
C21 C25 C26 C31 -77.0(4) . . . . ?
C21 C25 C26 C27 105.0(3) . . . . ?
C31 C26 C27 C28 -1.1(4) . . . . ?
C25 C26 C27 C28 177.0(3) . . . . ?
C26 C27 C28 C29 2.2(5) . . . . ?
C27 C28 C29 C30 -1.2(5) . . . . ?
C28 C29 C30 C31 -0.8(4) . . . . ?
C28 C29 C30 C32 -178.8(3) . . . . ?
C27 C26 C31 O4 177.2(3) . . . . ?
C25 C26 C31 O4 -0.8(4) . . . . ?
C27 C26 C31 C30 -1.0(4) . . . . ?
C25 C26 C31 C30 -179.1(3) . . . . ?
C29 C30 C31 O4 -176.2(3) . . . . ?
C32 C30 C31 O4 1.7(4) . . . . ?
C29 C30 C31 C26 2.0(4) . . . . ?
C32 C30 C31 C26 179.8(3) . . . . ?
C29 C30 C32 C1 -111.5(3) . . . . ?
C31 C30 C32 C1 70.7(4) . . . . ?
C6 C1 C32 C30 -97.0(3) . . . . ?
C2 C1 C32 C30 80.7(3) . . . . ?
C1 C6 O1 C7 -90.4(3) . . . . ?
C5 C6 O1 C7 92.6(3) . . . . ?
C8 C7 O1 C6 178.9(3) . . . . ?
C17 C22 O3 C23 -93.6(3) . . . . ?
C21 C22 O3 C23 89.4(3) . . . . ?
C24 C23 O3 C22 179.7(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O3 0.84 1.98 2.750(3) 151.0 .
O4 H4A O1 0.84 1.91 2.710(3) 157.8 .

_refine_diff_density_max         0.676
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.078

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
1 0.000 0.000 -0.007 321.4 64.8
2 0.333 0.667 0.206 322.6 64.9
3 0.667 0.333 0.873 322.7 64.9
_platon_squeeze_details          
;
;

_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_lcza110504
_database_code_depnum_ccdc_archive 'CCDC 1476806'
_audit_update_record             
;
2016-08-02 deposited with the CCDC.
2016-08-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H38 O4 S3'
_chemical_formula_sum            'C36 H38 O4 S3'
_chemical_formula_weight         630.84

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

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   10.2238(6)
_cell_length_b                   11.8889(7)
_cell_length_c                   14.4085(6)
_cell_angle_alpha                75.855(3)
_cell_angle_beta                 78.337(3)
_cell_angle_gamma                68.813(2)
_cell_volume                     1570.86(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7479
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    0.275
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_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      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15734
_diffrn_reflns_av_unetI/netI     0.1232
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.469
_diffrn_reflns_theta_max         27.590
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7185
_reflns_number_gt                3833
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'

_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)+(0.0923P)²+2.1697P] 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         7185
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1823
_refine_ls_R_factor_gt           0.0961
_refine_ls_wR_factor_ref         0.2429
_refine_ls_wR_factor_gt          0.1966
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
C1 C 0.5033(5) 0.2444(4) 0.8600(3) 0.0372(11) Uani 1 1 d . . . . .
C2 C 0.4786(5) 0.1339(5) 0.8972(3) 0.0423(12) Uani 1 1 d . . . . .
H2 H 0.4183 0.1258 0.9561 0.051 Uiso 1 1 calc R U . . .
C3 C 0.5400(5) 0.0350(5) 0.8503(3) 0.0418(12) Uani 1 1 d . . . . .
H3 H 0.5203 -0.0395 0.8761 0.050 Uiso 1 1 calc R U . . .
C4 C 0.6302(5) 0.0454(4) 0.7657(3) 0.0352(10) Uani 1 1 d . . . . .
H4 H 0.6746 -0.0235 0.7349 0.042 Uiso 1 1 calc R U . . .
C5 C 0.6573(4) 0.1541(4) 0.7248(3) 0.0296(10) Uani 1 1 d . . . . .
C6 C 0.5896(4) 0.2538(4) 0.7716(3) 0.0325(10) Uani 1 1 d . . . . .
C7 C 0.7619(5) 0.1610(4) 0.6348(3) 0.0365(11) Uani 1 1 d . . . . .
H7A H 0.7516 0.2483 0.6077 0.044 Uiso 1 1 calc R U . . .
H7B H 0.7389 0.1271 0.5863 0.044 Uiso 1 1 calc R U . . .
C8 C 0.9143(5) 0.0918(4) 0.6525(3) 0.0316(10) Uani 1 1 d . . . . .
C9 C 0.9860(5) -0.0210(5) 0.6265(3) 0.0395(11) Uani 1 1 d . . . . .
H9 H 0.9383 -0.0566 0.5978 0.047 Uiso 1 1 calc R U . . .
C10 C 1.1257(5) -0.0838(5) 0.6410(3) 0.0431(12) Uani 1 1 d . . . . .
H10 H 1.1746 -0.1603 0.6210 0.052 Uiso 1 1 calc R U . . .
C11 C 1.1927(5) -0.0325(5) 0.6854(3) 0.0392(11) Uani 1 1 d . . . . .
H11 H 1.2884 -0.0756 0.6959 0.047 Uiso 1 1 calc R U . . .
C12 C 1.1253(5) 0.0788(4) 0.7148(3) 0.0336(10) Uani 1 1 d . . . . .
C13 C 0.9850(5) 0.1419(4) 0.6968(3) 0.0311(10) Uani 1 1 d . . . . .
C14 C 1.2028(5) 0.1312(5) 0.7637(3) 0.0402(11) Uani 1 1 d . . . . .
H14A H 1.3050 0.0834 0.7563 0.048 Uiso 1 1 calc R U . . .
H14B H 1.1916 0.2171 0.7309 0.048 Uiso 1 1 calc R U . . .
C15 C 1.1500(5) 0.1290(4) 0.8705(3) 0.0357(11) Uani 1 1 d . . . . .
C16 C 1.1918(5) 0.0209(5) 0.9382(3) 0.0385(11) Uani 1 1 d . . . . .
H16 H 1.2559 -0.0518 0.9177 0.046 Uiso 1 1 calc R U . . .
C17 C 1.1410(5) 0.0185(5) 1.0348(3) 0.0421(12) Uani 1 1 d . . . . .
H17 H 1.1726 -0.0552 1.0804 0.050 Uiso 1 1 calc R U . . .
C18 C 1.0452(5) 0.1219(5) 1.0654(3) 0.0430(12) Uani 1 1 d . . . . .
H18 H 1.0105 0.1183 1.1320 0.052 Uiso 1 1 calc R U . . .
C19 C 0.9977(5) 0.2320(4) 1.0007(3) 0.0385(11) Uani 1 1 d . . . . .
C20 C 1.0572(5) 0.2330(4) 0.9037(3) 0.0357(11) Uani 1 1 d . . . . .
C21 C 0.8821(6) 0.3426(5) 1.0338(3) 0.0500(14) Uani 1 1 d . . . . .
H21A H 0.8797 0.4162 0.9831 0.060 Uiso 1 1 calc R U . . .
H21B H 0.9058 0.3559 1.0926 0.060 Uiso 1 1 calc R U . . .
C22 C 0.7360(5) 0.3293(4) 1.0553(3) 0.0408(12) Uani 1 1 d . . . . .
C23 C 0.6743(6) 0.3006(4) 1.1493(3) 0.0505(14) Uani 1 1 d . . . . .
H23 H 0.7243 0.2894 1.2015 0.061 Uiso 1 1 calc R U . . .
C24 C 0.5417(6) 0.2881(5) 1.1682(4) 0.0537(14) Uani 1 1 d . . . . .
H24 H 0.5008 0.2691 1.2329 0.064 Uiso 1 1 calc R U . . .
C25 C 0.4696(6) 0.3033(5) 1.0930(4) 0.0487(13) Uani 1 1 d . . . . .
H25 H 0.3788 0.2940 1.1065 0.058 Uiso 1 1 calc R U . . .
C26 C 0.5261(5) 0.3319(4) 0.9976(3) 0.0401(12) Uani 1 1 d . . . . .
C27 C 0.6589(5) 0.3458(4) 0.9791(3) 0.0391(11) Uani 1 1 d . . . . .
C28 C 0.4443(5) 0.3494(5) 0.9160(3) 0.0473(13) Uani 1 1 d . . . . .
H28A H 0.4449 0.4268 0.8709 0.057 Uiso 1 1 calc R U . . .
H28B H 0.3448 0.3576 0.9425 0.057 Uiso 1 1 calc R U . . .
C29 C 0.5206(5) 0.4521(4) 0.6692(3) 0.0399(11) Uani 1 1 d . . . . .
H29A H 0.4294 0.4927 0.7057 0.048 Uiso 1 1 calc R U . . .
H29B H 0.5025 0.4121 0.6226 0.048 Uiso 1 1 calc R U . . .
C30 C 0.5937(5) 0.5439(4) 0.6176(4) 0.0467(12) Uani 1 1 d . . . . .
H30A H 0.6686 0.5091 0.5671 0.056 Uiso 1 1 calc R U . . .
H30B H 0.6386 0.5630 0.6639 0.056 Uiso 1 1 calc R U . . .
C31 C 0.5752(6) 0.7695(6) 0.4885(4) 0.0621(16) Uani 1 1 d . . . . .
H31A H 0.6607 0.7118 0.4585 0.075 Uiso 1 1 calc R U . . .
H31B H 0.5223 0.8267 0.4358 0.075 Uiso 1 1 calc R U . . .
C32 C 0.6228(7) 0.8449(5) 0.5409(5) 0.0764(19) Uani 1 1 d . . . . .
H32A H 0.5387 0.8920 0.5800 0.092 Uiso 1 1 calc R U . . .
H32B H 0.6579 0.9050 0.4915 0.092 Uiso 1 1 calc R U . . .
C33 C 0.9005(6) 0.7150(7) 0.5271(4) 0.0709(18) Uani 1 1 d . . . . .
H33A H 0.8832 0.6575 0.4954 0.085 Uiso 1 1 calc R U . . .
H33B H 0.9028 0.7887 0.4776 0.085 Uiso 1 1 calc R U . . .
C34 C 1.0438(7) 0.6546(6) 0.5621(4) 0.0682(17) Uani 1 1 d . . . . .
H34A H 1.0572 0.7090 0.5988 0.082 Uiso 1 1 calc R U . . .
H34B H 1.1168 0.6482 0.5051 0.082 Uiso 1 1 calc R U . . .
C35 C 1.0369(8) 0.5379(5) 0.7556(4) 0.0674(18) Uani 1 1 d . . . . .
H35A H 1.0794 0.6001 0.7571 0.081 Uiso 1 1 calc R U . . .
H35B H 0.9334 0.5723 0.7729 0.081 Uiso 1 1 calc R U . . .
C36 C 1.0970(7) 0.4217(5) 0.8281(4) 0.0561(15) Uani 1 1 d . . . . .
H36A H 1.1973 0.3796 0.8056 0.067 Uiso 1 1 calc R U . . .
H36B H 1.0920 0.4426 0.8914 0.067 Uiso 1 1 calc R U . . .
O1 O 0.6160(3) 0.3640(3) 0.7333(2) 0.0380(8) Uani 1 1 d . . . . .
O2 O 0.9117(3) 0.2550(3) 0.7173(2) 0.0417(8) Uani 1 1 d . . . . .
H2O H 0.9643 0.2801 0.7389 0.063 Uiso 1 1 calc R U . . .
O3 O 1.0150(3) 0.3434(3) 0.8367(2) 0.0410(8) Uani 1 1 d . . . . .
O4 O 0.7226(4) 0.3784(3) 0.8892(2) 0.0449(8) Uani 1 1 d . . . . .
H4O H 0.6765 0.3766 0.8479 0.067 Uiso 1 1 calc R U . . .
S1 S 0.46588(14) 0.68230(13) 0.56348(9) 0.0508(4) Uani 1 1 d . . . . .
S2 S 0.75587(16) 0.75983(14) 0.61776(10) 0.0564(4) Uani 1 1 d . . . . .
S3 S 1.0742(2) 0.50360(14) 0.63713(10) 0.0686(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.385(7) . ?
C1 C6 1.401(6) . ?
C1 C28 1.524(6) . ?
C2 C3 1.384(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(6) . ?
C5 C7 1.511(6) . ?
C6 O1 1.391(5) . ?
C7 C8 1.518(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.380(6) . ?
C8 C13 1.403(6) . ?
C9 C10 1.384(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.385(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.401(6) . ?
C12 C14 1.521(6) . ?
C13 O2 1.354(5) . ?
C14 C15 1.521(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.385(6) . ?
C15 C16 1.395(7) . ?
C16 C17 1.381(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.373(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.395(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(6) . ?
C19 C21 1.519(7) . ?
C20 O3 1.407(5) . ?
C21 C22 1.520(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.390(7) . ?
C22 C27 1.413(6) . ?
C23 C24 1.382(8) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.391(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.391(7) . ?
C26 C28 1.510(7) . ?
C27 O4 1.359(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O1 1.434(5) . ?
C29 C30 1.507(7) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 S1 1.804(5) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.550(9) . ?
C31 S1 1.815(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 S2 1.779(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.509(8) . ?
C33 S2 1.779(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 S3 1.809(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.522(8) . ?
C35 S3 1.785(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 O3 1.432(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
O2 H2O 0.8400 . ?
O4 H4O 0.8400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 117.5(4) . . ?
C2 C1 C28 120.9(4) . . ?
C6 C1 C28 121.5(4) . . ?
C3 C2 C1 121.4(4) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C4 C3 C2 119.6(5) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 121.4(4) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C6 117.8(4) . . ?
C4 C5 C7 120.2(4) . . ?
C6 C5 C7 121.9(4) . . ?
O1 C6 C5 119.4(4) . . ?
O1 C6 C1 118.3(4) . . ?
C5 C6 C1 122.1(4) . . ?
C5 C7 C8 113.3(3) . . ?
C5 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C5 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C13 118.6(4) . . ?
C9 C8 C7 121.3(4) . . ?
C13 C8 C7 120.1(4) . . ?
C8 C9 C10 121.6(4) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C9 C10 C11 118.6(4) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 122.3(4) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C13 118.0(4) . . ?
C11 C12 C14 120.5(4) . . ?
C13 C12 C14 121.6(4) . . ?
O2 C13 C12 122.9(4) . . ?
O2 C13 C8 116.1(4) . . ?
C12 C13 C8 120.9(4) . . ?
C15 C14 C12 113.2(4) . . ?
C15 C14 H14A 108.9 . . ?
C12 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
C12 C14 H14B 108.9 . . ?
H14A C14 H14B 107.8 . . ?
C20 C15 C16 117.7(4) . . ?
C20 C15 C14 121.5(4) . . ?
C16 C15 C14 120.9(4) . . ?
C17 C16 C15 120.7(5) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C18 C17 C16 120.4(5) . . ?
C18 C17 H17 119.8 . . ?
C16 C17 H17 119.8 . . ?
C17 C18 C19 121.4(4) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 H18 119.3 . . ?
C18 C19 C20 116.7(4) . . ?
C18 C19 C21 121.0(4) . . ?
C20 C19 C21 122.3(4) . . ?
C15 C20 C19 122.9(4) . . ?
C15 C20 O3 118.6(4) . . ?
C19 C20 O3 118.4(4) . . ?
C19 C21 C22 113.6(4) . . ?
C19 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
C19 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C27 118.0(5) . . ?
C23 C22 C21 121.6(4) . . ?
C27 C22 C21 120.3(4) . . ?
C24 C23 C22 121.3(5) . . ?
C24 C23 H23 119.3 . . ?
C22 C23 H23 119.3 . . ?
C25 C24 C23 119.5(5) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 121.7(5) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C27 118.5(4) . . ?
C25 C26 C28 120.8(5) . . ?
C27 C26 C28 120.8(4) . . ?
O4 C27 C26 123.9(4) . . ?
O4 C27 C22 115.1(4) . . ?
C26 C27 C22 121.0(4) . . ?
C26 C28 C1 113.5(4) . . ?
C26 C28 H28A 108.9 . . ?
C1 C28 H28A 108.9 . . ?
C26 C28 H28B 108.9 . . ?
C1 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
O1 C29 C30 105.3(4) . . ?
O1 C29 H29A 110.7 . . ?
C30 C29 H29A 110.7 . . ?
O1 C29 H29B 110.7 . . ?
C30 C29 H29B 110.7 . . ?
H29A C29 H29B 108.8 . . ?
C29 C30 S1 109.3(3) . . ?
C29 C30 H30A 109.8 . . ?
S1 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
S1 C30 H30B 109.8 . . ?
H30A C30 H30B 108.3 . . ?
C32 C31 S1 115.7(4) . . ?
C32 C31 H31A 108.4 . . ?
S1 C31 H31A 108.4 . . ?
C32 C31 H31B 108.4 . . ?
S1 C31 H31B 108.4 . . ?
H31A C31 H31B 107.4 . . ?
C31 C32 S2 116.4(4) . . ?
C31 C32 H32A 108.2 . . ?
S2 C32 H32A 108.2 . . ?
C31 C32 H32B 108.2 . . ?
S2 C32 H32B 108.2 . . ?
H32A C32 H32B 107.3 . . ?
C34 C33 S2 115.4(4) . . ?
C34 C33 H33A 108.4 . . ?
S2 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
S2 C33 H33B 108.4 . . ?
H33A C33 H33B 107.5 . . ?
C33 C34 S3 116.1(5) . . ?
C33 C34 H34A 108.3 . . ?
S3 C34 H34A 108.3 . . ?
C33 C34 H34B 108.3 . . ?
S3 C34 H34B 108.3 . . ?
H34A C34 H34B 107.4 . . ?
C36 C35 S3 109.9(4) . . ?
C36 C35 H35A 109.7 . . ?
S3 C35 H35A 109.7 . . ?
C36 C35 H35B 109.7 . . ?
S3 C35 H35B 109.7 . . ?
H35A C35 H35B 108.2 . . ?
O3 C36 C35 108.0(4) . . ?
O3 C36 H36A 110.1 . . ?
C35 C36 H36A 110.1 . . ?
O3 C36 H36B 110.1 . . ?
C35 C36 H36B 110.1 . . ?
H36A C36 H36B 108.4 . . ?
C6 O1 C29 116.2(3) . . ?
C13 O2 H2O 109.5 . . ?
C20 O3 C36 114.0(3) . . ?
C27 O4 H4O 109.5 . . ?
C30 S1 C31 103.0(3) . . ?
C32 S2 C33 98.2(3) . . ?
C35 S3 C34 102.0(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.8(6) . . . . ?
C28 C1 C2 C3 -175.3(4) . . . . ?
C1 C2 C3 C4 1.4(7) . . . . ?
C2 C3 C4 C5 -2.1(7) . . . . ?
C3 C4 C5 C6 -0.4(6) . . . . ?
C3 C4 C5 C7 177.1(4) . . . . ?
C4 C5 C6 O1 179.1(4) . . . . ?
C7 C5 C6 O1 1.6(6) . . . . ?
C4 C5 C6 C1 3.8(6) . . . . ?
C7 C5 C6 C1 -173.7(4) . . . . ?
C2 C1 C6 O1 -179.8(4) . . . . ?
C28 C1 C6 O1 -2.7(6) . . . . ?
C2 C1 C6 C5 -4.4(6) . . . . ?
C28 C1 C6 C5 172.6(4) . . . . ?
C4 C5 C7 C8 -71.5(5) . . . . ?
C6 C5 C7 C8 105.8(5) . . . . ?
C5 C7 C8 C9 103.4(5) . . . . ?
C5 C7 C8 C13 -76.2(5) . . . . ?
C13 C8 C9 C10 -1.5(7) . . . . ?
C7 C8 C9 C10 179.0(4) . . . . ?
C8 C9 C10 C11 1.8(7) . . . . ?
C9 C10 C11 C12 -0.4(7) . . . . ?
C10 C11 C12 C13 -1.2(7) . . . . ?
C10 C11 C12 C14 179.7(4) . . . . ?
C11 C12 C13 O2 -175.9(4) . . . . ?
C14 C12 C13 O2 3.2(6) . . . . ?
C11 C12 C13 C8 1.6(6) . . . . ?
C14 C12 C13 C8 -179.3(4) . . . . ?
C9 C8 C13 O2 177.4(4) . . . . ?
C7 C8 C13 O2 -3.1(6) . . . . ?
C9 C8 C13 C12 -0.3(6) . . . . ?
C7 C8 C13 C12 179.3(4) . . . . ?
C11 C12 C14 C15 -109.4(5) . . . . ?
C13 C12 C14 C15 71.5(6) . . . . ?
C12 C14 C15 C20 -100.2(5) . . . . ?
C12 C14 C15 C16 78.7(5) . . . . ?
C20 C15 C16 C17 0.4(6) . . . . ?
C14 C15 C16 C17 -178.4(4) . . . . ?
C15 C16 C17 C18 1.9(7) . . . . ?
C16 C17 C18 C19 -0.7(7) . . . . ?
C17 C18 C19 C20 -2.6(6) . . . . ?
C17 C18 C19 C21 174.5(4) . . . . ?
C16 C15 C20 C19 -4.0(6) . . . . ?
C14 C15 C20 C19 174.9(4) . . . . ?
C16 C15 C20 O3 179.3(4) . . . . ?
C14 C15 C20 O3 -1.9(6) . . . . ?
C18 C19 C20 C15 5.1(6) . . . . ?
C21 C19 C20 C15 -172.0(4) . . . . ?
C18 C19 C20 O3 -178.2(4) . . . . ?
C21 C19 C20 O3 4.7(6) . . . . ?
C18 C19 C21 C22 -72.5(5) . . . . ?
C20 C19 C21 C22 104.4(5) . . . . ?
C19 C21 C22 C23 102.5(5) . . . . ?
C19 C21 C22 C27 -77.5(6) . . . . ?
C27 C22 C23 C24 0.2(7) . . . . ?
C21 C22 C23 C24 -179.7(5) . . . . ?
C22 C23 C24 C25 0.5(8) . . . . ?
C23 C24 C25 C26 -0.5(8) . . . . ?
C24 C25 C26 C27 -0.3(7) . . . . ?
C24 C25 C26 C28 -179.4(5) . . . . ?
C25 C26 C27 O4 -177.3(4) . . . . ?
C28 C26 C27 O4 1.8(7) . . . . ?
C25 C26 C27 C22 1.1(7) . . . . ?
C28 C26 C27 C22 -179.8(4) . . . . ?
C23 C22 C27 O4 177.5(4) . . . . ?
C21 C22 C27 O4 -2.6(6) . . . . ?
C23 C22 C27 C26 -1.0(7) . . . . ?
C21 C22 C27 C26 178.9(4) . . . . ?
C25 C26 C28 C1 -107.6(5) . . . . ?
C27 C26 C28 C1 73.4(6) . . . . ?
C2 C1 C28 C26 77.0(6) . . . . ?
C6 C1 C28 C26 -99.9(5) . . . . ?
O1 C29 C30 S1 -162.5(3) . . . . ?
S1 C31 C32 S2 73.4(5) . . . . ?
S2 C33 C34 S3 68.7(6) . . . . ?
S3 C35 C36 O3 -69.9(6) . . . . ?
C5 C6 O1 C29 93.0(5) . . . . ?
C1 C6 O1 C29 -91.5(5) . . . . ?
C30 C29 O1 C6 -164.6(4) . . . . ?
C15 C20 O3 C36 -95.1(5) . . . . ?
C19 C20 O3 C36 88.0(5) . . . . ?
C35 C36 O3 C20 -178.6(4) . . . . ?
C29 C30 S1 C31 -170.4(4) . . . . ?
C32 C31 S1 C30 -82.9(5) . . . . ?
C31 C32 S2 C33 70.4(5) . . . . ?
C34 C33 S2 C32 171.1(5) . . . . ?
C36 C35 S3 C34 -163.5(4) . . . . ?
C33 C34 S3 C35 -97.2(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2O O3 0.84 1.98 2.757(4) 153.8 .
O4 H4O O1 0.84 1.93 2.753(4) 165.6 .

_refine_diff_density_max         0.636
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.098

_shelxl_version_number           2013-4

