# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_AJ_a
_database_code_depnum_ccdc_archive 'CCDC 1975421'
loop_
_audit_author_name
_audit_author_address
'ANOOP KUMAR PANDAY'
;Indian Institute of Technology Patna, Patna
India
;
_audit_update_record             
;
2020-01-04 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H15 Cl O4 S'
_chemical_formula_sum            'C23 H15 Cl O4 S'
_chemical_formula_weight         422.86

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'
Cl Cl 0.1484 0.1585 '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                   8.7831(8)
_cell_length_b                   8.9008(7)
_cell_length_c                   13.3834(12)
_cell_angle_alpha                99.835(2)
_cell_angle_beta                 100.128(2)
_cell_angle_gamma                106.436(2)
_cell_volume                     960.54(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.15

_exptl_crystal_description       CUBE
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_F_000             436
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.336
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.906
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26141
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.489
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3571
_reflns_number_gt                2945
_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-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+0.5229P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0094(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3571
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1010
_refine_ls_wR_factor_gt          0.0938
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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 0.5550(3) 0.9063(3) 0.82848(18) 0.0510(5) Uani 1 1 d . . . . .
H1 H 0.4800 0.9254 0.7780 0.061 Uiso 1 1 calc R U . . .
C2 C 0.6397(3) 1.0249(3) 0.9160(2) 0.0624(6) Uani 1 1 d . . . . .
H2 H 0.6203 1.1231 0.9255 0.075 Uiso 1 1 calc R U . . .
C3 C 0.7526(3) 0.9998(3) 0.9894(2) 0.0692(7) Uani 1 1 d . . . . .
H3 H 0.8106 1.0815 1.0485 0.083 Uiso 1 1 calc R U . . .
C4 C 0.7816(3) 0.8544(3) 0.97677(19) 0.0661(7) Uani 1 1 d . . . . .
H4 H 0.8597 0.8386 1.0268 0.079 Uiso 1 1 calc R U . . .
C5 C 0.6951(3) 0.7327(3) 0.89033(17) 0.0509(5) Uani 1 1 d . . . . .
H5 H 0.7133 0.6339 0.8825 0.061 Uiso 1 1 calc R U . . .
C6 C 0.5800(2) 0.7572(2) 0.81425(15) 0.0401(4) Uani 1 1 d . . . . .
C7 C 0.4779(2) 0.6316(2) 0.72095(15) 0.0405(4) Uani 1 1 d . . . . .
C8 C 0.4692(2) 0.4569(2) 0.71391(15) 0.0376(4) Uani 1 1 d . . . . .
H6 H 0.5240 0.4510 0.7829 0.045 Uiso 1 1 calc R U . . .
C9 C 0.7826(2) 0.4454(2) 0.71002(15) 0.0418(5) Uani 1 1 d . . . . .
C10 C 0.9168(2) 0.5696(3) 0.70671(16) 0.0452(5) Uani 1 1 d . . . . .
H7 H 0.9065 0.6315 0.6581 0.054 Uiso 1 1 calc R U . . .
C11 C 1.0661(2) 0.6028(3) 0.77500(16) 0.0463(5) Uani 1 1 d . . . . .
H8 H 1.1563 0.6863 0.7725 0.056 Uiso 1 1 calc R U . . .
C12 C 1.0796(2) 0.5106(2) 0.84669(16) 0.0427(5) Uani 1 1 d . . . . .
C13 C 0.9479(3) 0.3862(3) 0.85087(18) 0.0509(5) Uani 1 1 d . . . . .
H9 H 0.9585 0.3248 0.8998 0.061 Uiso 1 1 calc R U . . .
C14 C 0.7996(3) 0.3532(3) 0.78172(18) 0.0507(5) Uani 1 1 d . . . . .
H10 H 0.7103 0.2681 0.7835 0.061 Uiso 1 1 calc R U . . .
C15 C 0.3000(2) 0.3346(2) 0.68658(15) 0.0367(4) Uani 1 1 d . . . . .
C16 C 0.1711(2) 0.3195(2) 0.60859(14) 0.0386(4) Uani 1 1 d . . . . .
C17 C 0.0164(2) 0.1931(2) 0.59211(15) 0.0414(5) Uani 1 1 d . . . . .
C18 C -0.1219(3) 0.1731(3) 0.51493(18) 0.0517(5) Uani 1 1 d . . . . .
H12 H -0.1172 0.2411 0.4691 0.062 Uiso 1 1 calc R U . . .
C19 C -0.2653(3) 0.0529(3) 0.5067(2) 0.0638(7) Uani 1 1 d . . . . .
H13 H -0.3566 0.0386 0.4543 0.077 Uiso 1 1 calc R U . . .
C20 C -0.2745(3) -0.0460(3) 0.5752(2) 0.0666(7) Uani 1 1 d . . . . .
H14 H -0.3727 -0.1257 0.5694 0.080 Uiso 1 1 calc R U . . .
C21 C -0.1412(3) -0.0287(3) 0.6518(2) 0.0606(6) Uani 1 1 d . . . . .
H15 H -0.1482 -0.0954 0.6985 0.073 Uiso 1 1 calc R U . . .
C22 C 0.0046(2) 0.0900(2) 0.65891(17) 0.0460(5) Uani 1 1 d . . . . .
C23 C 0.2862(2) 0.2145(2) 0.74916(17) 0.0441(5) Uani 1 1 d . . . . .
Cl1 Cl 1.26771(7) 0.55119(8) 0.93247(5) 0.0623(2) Uani 1 1 d . . . . .
O1 O 0.39920(19) 0.66879(18) 0.64912(12) 0.0576(4) Uani 1 1 d . . . . .
O2 O 0.17187(18) 0.41416(19) 0.54186(11) 0.0534(4) Uani 1 1 d . . . . .
H11 H 0.2439 0.5010 0.5676 0.080 Uiso 1 1 calc R U . . .
O3 O 0.13614(18) 0.10098(17) 0.73538(12) 0.0536(4) Uani 1 1 d . . . . .
O4 O 0.3965(2) 0.2070(2) 0.81334(14) 0.0661(5) Uani 1 1 d . . . . .
S1 S 0.59169(6) 0.40622(8) 0.62218(4) 0.0578(2) 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 1.366(3) . ?
C1 C6 1.393(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.362(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.475(3) . ?
C7 O1 1.232(2) . ?
C7 C8 1.521(3) . ?
C8 C15 1.511(3) . ?
C8 S1 1.8488(19) . ?
C8 H6 0.9800 . ?
C9 C14 1.380(3) . ?
C9 C10 1.383(3) . ?
C9 S1 1.775(2) . ?
C10 C11 1.382(3) . ?
C10 H7 0.9300 . ?
C11 C12 1.376(3) . ?
C11 H8 0.9300 . ?
C12 C13 1.373(3) . ?
C12 Cl1 1.741(2) . ?
C13 C14 1.381(3) . ?
C13 H9 0.9300 . ?
C14 H10 0.9300 . ?
C15 C16 1.356(3) . ?
C15 C23 1.459(3) . ?
C16 O2 1.328(2) . ?
C16 C17 1.451(3) . ?
C17 C22 1.382(3) . ?
C17 C18 1.396(3) . ?
C18 C19 1.375(3) . ?
C18 H12 0.9300 . ?
C19 C20 1.373(4) . ?
C19 H13 0.9300 . ?
C20 C21 1.367(4) . ?
C20 H14 0.9300 . ?
C21 C22 1.387(3) . ?
C21 H15 0.9300 . ?
C22 O3 1.370(3) . ?
C23 O4 1.201(2) . ?
C23 O3 1.375(2) . ?
O2 H11 0.8200 . ?

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 120.5(2) . . ?
C2 C1 H1 119.7 . . ?
C6 C1 H1 119.7 . . ?
C3 C2 C1 120.3(2) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 120.4(2) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 120.1(2) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 118.55(19) . . ?
C1 C6 C7 117.77(19) . . ?
C5 C6 C7 123.64(18) . . ?
O1 C7 C6 119.65(18) . . ?
O1 C7 C8 120.24(18) . . ?
C6 C7 C8 120.10(17) . . ?
C15 C8 C7 116.31(15) . . ?
C15 C8 S1 111.53(13) . . ?
C7 C8 S1 107.93(13) . . ?
C15 C8 H6 106.9 . . ?
C7 C8 H6 106.9 . . ?
S1 C8 H6 106.9 . . ?
C14 C9 C10 119.28(19) . . ?
C14 C9 S1 120.95(16) . . ?
C10 C9 S1 119.78(16) . . ?
C11 C10 C9 120.6(2) . . ?
C11 C10 H7 119.7 . . ?
C9 C10 H7 119.7 . . ?
C12 C11 C10 119.07(19) . . ?
C12 C11 H8 120.5 . . ?
C10 C11 H8 120.5 . . ?
C13 C12 C11 121.16(19) . . ?
C13 C12 Cl1 119.58(17) . . ?
C11 C12 Cl1 119.25(16) . . ?
C12 C13 C14 119.3(2) . . ?
C12 C13 H9 120.3 . . ?
C14 C13 H9 120.3 . . ?
C9 C14 C13 120.54(19) . . ?
C9 C14 H10 119.7 . . ?
C13 C14 H10 119.7 . . ?
C16 C15 C23 119.26(18) . . ?
C16 C15 C8 127.85(17) . . ?
C23 C15 C8 112.68(16) . . ?
O2 C16 C15 125.04(18) . . ?
O2 C16 C17 114.12(17) . . ?
C15 C16 C17 120.85(18) . . ?
C22 C17 C18 118.38(19) . . ?
C22 C17 C16 117.86(18) . . ?
C18 C17 C16 123.73(19) . . ?
C19 C18 C17 120.0(2) . . ?
C19 C18 H12 120.0 . . ?
C17 C18 H12 120.0 . . ?
C20 C19 C18 120.5(2) . . ?
C20 C19 H13 119.8 . . ?
C18 C19 H13 119.8 . . ?
C21 C20 C19 120.8(2) . . ?
C21 C20 H14 119.6 . . ?
C19 C20 H14 119.6 . . ?
C20 C21 C22 118.9(2) . . ?
C20 C21 H15 120.6 . . ?
C22 C21 H15 120.6 . . ?
O3 C22 C17 121.53(18) . . ?
O3 C22 C21 117.0(2) . . ?
C17 C22 C21 121.5(2) . . ?
O4 C23 O3 116.57(18) . . ?
O4 C23 C15 125.05(19) . . ?
O3 C23 C15 118.38(17) . . ?
C16 O2 H11 109.5 . . ?
C22 O3 C23 121.69(16) . . ?
C9 S1 C8 100.80(9) . . ?

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 1.5(4) . . . . ?
C1 C2 C3 C4 -0.6(4) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C3 C4 C5 C6 1.2(4) . . . . ?
C2 C1 C6 C5 -1.1(3) . . . . ?
C2 C1 C6 C7 176.6(2) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
C4 C5 C6 C7 -177.8(2) . . . . ?
C1 C6 C7 O1 14.4(3) . . . . ?
C5 C6 C7 O1 -168.0(2) . . . . ?
C1 C6 C7 C8 -165.17(18) . . . . ?
C5 C6 C7 C8 12.4(3) . . . . ?
O1 C7 C8 C15 -51.0(3) . . . . ?
C6 C7 C8 C15 128.58(18) . . . . ?
O1 C7 C8 S1 75.2(2) . . . . ?
C6 C7 C8 S1 -105.24(17) . . . . ?
C14 C9 C10 C11 -0.7(3) . . . . ?
S1 C9 C10 C11 179.48(15) . . . . ?
C9 C10 C11 C12 -0.1(3) . . . . ?
C10 C11 C12 C13 0.4(3) . . . . ?
C10 C11 C12 Cl1 179.68(15) . . . . ?
C11 C12 C13 C14 0.1(3) . . . . ?
Cl1 C12 C13 C14 -179.14(16) . . . . ?
C10 C9 C14 C13 1.2(3) . . . . ?
S1 C9 C14 C13 -178.93(16) . . . . ?
C12 C13 C14 C9 -1.0(3) . . . . ?
C7 C8 C15 C16 47.8(3) . . . . ?
S1 C8 C15 C16 -76.5(2) . . . . ?
C7 C8 C15 C23 -137.47(17) . . . . ?
S1 C8 C15 C23 98.17(16) . . . . ?
C23 C15 C16 O2 -175.25(18) . . . . ?
C8 C15 C16 O2 -0.9(3) . . . . ?
C23 C15 C16 C17 4.8(3) . . . . ?
C8 C15 C16 C17 179.21(17) . . . . ?
O2 C16 C17 C22 -179.38(17) . . . . ?
C15 C16 C17 C22 0.6(3) . . . . ?
O2 C16 C17 C18 -1.5(3) . . . . ?
C15 C16 C17 C18 178.48(18) . . . . ?
C22 C17 C18 C19 -0.1(3) . . . . ?
C16 C17 C18 C19 -178.04(19) . . . . ?
C17 C18 C19 C20 1.3(3) . . . . ?
C18 C19 C20 C21 -1.0(4) . . . . ?
C19 C20 C21 C22 -0.5(4) . . . . ?
C18 C17 C22 O3 178.96(18) . . . . ?
C16 C17 C22 O3 -3.0(3) . . . . ?
C18 C17 C22 C21 -1.4(3) . . . . ?
C16 C17 C22 C21 176.65(19) . . . . ?
C20 C21 C22 O3 -178.62(19) . . . . ?
C20 C21 C22 C17 1.7(3) . . . . ?
C16 C15 C23 O4 172.7(2) . . . . ?
C8 C15 C23 O4 -2.5(3) . . . . ?
C16 C15 C23 O3 -8.0(3) . . . . ?
C8 C15 C23 O3 176.86(16) . . . . ?
C17 C22 O3 C23 -0.3(3) . . . . ?
C21 C22 O3 C23 -179.92(18) . . . . ?
O4 C23 O3 C22 -174.87(19) . . . . ?
C15 C23 O3 C22 5.7(3) . . . . ?
C14 C9 S1 C8 66.04(18) . . . . ?
C10 C9 S1 C8 -114.13(16) . . . . ?
C15 C8 S1 C9 -137.20(14) . . . . ?
C7 C8 S1 C9 93.86(14) . . . . ?

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.039

####################################################################### 
# 
# 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_asim
_database_code_depnum_ccdc_archive 'CCDC 1975422'
loop_
_audit_author_name
_audit_author_address
'ANOOP KUMAR PANDAY'
;Indian Institute of Technology Patna, Patna
India
;
_audit_update_record             
;
2020-01-04 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C34 H20 O7), C2 H6 O S, C2 H6 O S0.21, 0.791(S)'
_chemical_formula_sum            'C72 H52 O16 S2'
_chemical_formula_weight         1237.26

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                   13.7724(13)
_cell_length_b                   15.3172(15)
_cell_length_c                   15.8809(15)
_cell_angle_alpha                80.591(2)
_cell_angle_beta                 65.912(2)
_cell_angle_gamma                82.455(2)
_cell_volume                     3009.5(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8367
_cell_measurement_theta_min      2.541
_cell_measurement_theta_max      18.874

_exptl_crystal_description       NEEDLELIKE
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             1288
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.162
_shelx_estimated_absorpt_T_min   0.953
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25696
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.541
_diffrn_reflns_theta_max         18.874
_diffrn_reflns_theta_full        18.874
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4753
_reflns_number_gt                3647
_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-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0454P)²+2.3442P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4736
_refine_ls_number_parameters     865
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0907
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.038
_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
C57 C 0.1955(3) -0.0543(2) 0.5548(3) 0.0323(10) Uani 1 1 d . . . A 4
C56 C 0.0867(3) -0.0449(3) 0.6277(3) 0.0300(10) Uani 1 1 d . . . A 4
C64 C 0.3262(3) -0.0951(3) 0.4061(3) 0.0358(10) Uani 1 1 d . . . A 4
C47 C 0.0789(3) 0.1247(3) 0.6166(3) 0.0313(10) Uani 1 1 d . . . A 4
C45 C -0.0632(3) 0.0210(3) 0.7242(3) 0.0330(10) Uani 1 1 d . . . A 4
C13 C 0.4339(3) 0.4095(3) 0.8326(3) 0.0368(11) Uani 1 1 d . . . B 4
C46 C 0.0341(3) 0.0381(3) 0.6574(3) 0.0322(10) Uani 1 1 d . . . A 4
C11 C 0.6027(3) 0.4955(3) 0.7571(3) 0.0343(10) Uani 1 1 d . . . B 4
C66 C 0.0189(3) -0.1087(3) 0.6790(3) 0.0340(10) Uani 1 1 d . . . A 4
C54 C 0.1514(3) 0.2600(3) 0.6188(3) 0.0345(10) Uani 1 1 d . . . A 4
C67 C 0.0233(4) -0.2054(3) 0.6852(3) 0.0369(10) Uani 1 1 d . . . A 4
C23 C 0.3434(3) 0.5870(2) 0.9139(3) 0.0368(11) Uani 1 1 d . . . B 4
C48 C 0.0925(3) 0.1533(3) 0.5218(3) 0.0345(10) Uani 1 1 d . . . A 4
C49 C 0.1590(3) 0.2879(3) 0.5294(3) 0.0379(11) Uani 1 1 d . . . A 4
C10 C 0.6918(3) 0.4391(3) 0.7017(3) 0.0366(10) Uani 1 1 d . . . B 4
C55 C 0.1126(3) 0.1743(3) 0.6618(3) 0.0376(11) Uani 1 1 d . . . A 4
C12 C 0.4978(3) 0.4870(3) 0.8110(3) 0.0342(10) Uani 1 1 d . . . B 4
C44 C -0.1565(3) 0.0737(3) 0.7815(3) 0.0380(11) Uani 1 1 d . . . A 4
C14 C 0.3974(3) 0.3927(3) 0.7638(3) 0.0447(12) Uani 1 1 d . . . B 4
C58 C 0.2792(3) -0.0224(3) 0.5710(3) 0.0446(11) Uani 1 1 d . . . A 4
C9 C 0.6790(3) 0.3792(3) 0.6514(3) 0.0503(12) Uani 1 1 d . . . B 4
H9 H 0.6109 0.3706 0.6569 0.060 Uiso 1 1 calc R U . B 4
C21 C 0.4004(3) 0.3610(3) 0.9167(3) 0.0440(11) Uani 1 1 d . . . B 4
C5 C 0.7936(4) 0.4486(3) 0.6938(3) 0.0482(12) Uani 1 1 d . . . B 4
H5 H 0.8035 0.4875 0.7284 0.058 Uiso 1 1 calc R U . B 4
C25 C 0.1346(4) 0.5948(3) 1.0479(4) 0.0487(12) Uani 1 1 d . . . B 4
C68 C 0.1199(4) -0.2554(3) 0.6565(3) 0.0536(12) Uani 1 1 d . . . A 4
H68 H 0.1831 -0.2272 0.6336 0.064 Uiso 1 1 calc R U . A 4
C50 C 0.1918(3) 0.3705(3) 0.4841(3) 0.0552(12) Uani 1 1 d . . . A 4
H50 H 0.1961 0.3881 0.4239 0.066 Uiso 1 1 calc R U . A 4
C63 C 0.3582(4) -0.1354(3) 0.3249(3) 0.0476(12) Uani 1 1 d . . . A 4
H63 H 0.3073 -0.1576 0.3112 0.057 Uiso 1 1 calc R U . A 4
C43 C -0.1559(3) 0.1641(3) 0.7802(3) 0.0508(12) Uani 1 1 d . . . A 4
H43 H -0.0942 0.1921 0.7420 0.061 Uiso 1 1 calc R U . A 4
C53 C 0.1800(3) 0.3177(3) 0.6625(3) 0.0531(12) Uani 1 1 d . . . A 4
H53 H 0.1764 0.3006 0.7226 0.064 Uiso 1 1 calc R U . A 4
C8 C 0.7664(5) 0.3318(3) 0.5927(3) 0.0591(13) Uani 1 1 d . . . B 4
H8 H 0.7567 0.2920 0.5588 0.071 Uiso 1 1 calc R U . B 4
C16 C 0.2305(4) 0.2092(3) 0.8877(4) 0.0579(13) Uani 1 1 d . . . B 4
H16 H 0.2135 0.1975 0.8399 0.070 Uiso 1 1 calc R U . B 4
C39 C -0.2503(4) 0.0350(3) 0.8402(3) 0.0579(13) Uani 1 1 d . . . A 4
H39 H -0.2544 -0.0256 0.8430 0.069 Uiso 1 1 calc R U . A 4
C60 C 0.5103(4) -0.0678(3) 0.3625(4) 0.0597(13) Uani 1 1 d . . . A 4
H60 H 0.5612 -0.0438 0.3747 0.072 Uiso 1 1 calc R U . A 4
C38 C 0.6425(4) 0.7564(3) 0.7505(3) 0.0554(12) Uani 1 1 d . . . B 4
H38 H 0.6993 0.7210 0.7137 0.066 Uiso 1 1 calc R U . B 4
C72 C -0.0682(4) -0.2498(3) 0.7208(3) 0.0598(13) Uani 1 1 d . . . A 4
H72 H -0.1342 -0.2180 0.7417 0.072 Uiso 1 1 calc R U . A 4
C6 C 0.8809(4) 0.4013(3) 0.6354(3) 0.0611(13) Uani 1 1 d . . . B 4
H6 H 0.9491 0.4087 0.6305 0.073 Uiso 1 1 calc R U . B 4
C42 C -0.2437(4) 0.2141(3) 0.8336(3) 0.0590(13) Uani 1 1 d . . . A 4
H42 H -0.2406 0.2749 0.8303 0.071 Uiso 1 1 calc R U . A 4
C62 C 0.4635(4) -0.1427(3) 0.2654(3) 0.0594(13) Uani 1 1 d . . . A 4
H62 H 0.4839 -0.1707 0.2124 0.071 Uiso 1 1 calc R U . A 4
C41 C -0.3350(4) 0.1749(4) 0.8910(3) 0.0642(14) Uani 1 1 d . . . A 4
H41 H -0.3944 0.2084 0.9272 0.077 Uiso 1 1 calc R U . A 4
C51 C 0.2180(4) 0.4257(3) 0.5299(4) 0.0642(14) Uani 1 1 d . . . A 4
H51 H 0.2395 0.4818 0.5008 0.077 Uiso 1 1 calc R U . A 4
C52 C 0.2131(4) 0.3992(3) 0.6184(4) 0.0616(13) Uani 1 1 d . . . A 4
H52 H 0.2324 0.4370 0.6483 0.074 Uiso 1 1 calc R U . A 4
C34 C 0.4673(4) 0.7727(3) 0.8645(3) 0.0634(13) Uani 1 1 d . . . B 4
H34 H 0.4040 0.7488 0.9062 0.076 Uiso 1 1 calc R U . B 4
C26 C 0.0339(5) 0.5965(3) 1.1182(3) 0.0656(14) Uani 1 1 d . . . B 4
H26 H 0.0247 0.5910 1.1802 0.079 Uiso 1 1 calc R U . B 4
C17 C 0.1894(4) 0.1630(3) 0.9728(5) 0.0780(16) Uani 1 1 d . . . B 4
H17 H 0.1444 0.1184 0.9838 0.094 Uiso 1 1 calc R U . B 4
C35 C 0.4783(4) 0.8619(4) 0.8574(4) 0.0755(15) Uani 1 1 d . . . B 4
H35 H 0.4220 0.8976 0.8942 0.091 Uiso 1 1 calc R U . B 4
C19 C 0.2842(4) 0.2441(4) 1.0274(4) 0.0724(15) Uani 1 1 d . . . B 4
H19 H 0.3027 0.2545 1.0749 0.087 Uiso 1 1 calc R U . B 4
C71 C -0.0636(5) -0.3412(4) 0.7262(4) 0.0758(15) Uani 1 1 d . . . A 4
H71 H -0.1263 -0.3703 0.7510 0.091 Uiso 1 1 calc R U . A 4
C18 C 0.2138(5) 0.1815(4) 1.0436(4) 0.0904(18) Uani 1 1 d . . . B 4
H18 H 0.1824 0.1513 1.1029 0.108 Uiso 1 1 calc R U . B 4
C22 C 0.4550(3) 0.5703(3) 0.8483(3) 0.0362(10) Uani 1 1 d . . . B 4
C33 C 0.5493(4) 0.7182(3) 0.8104(3) 0.0409(11) Uani 1 1 d . . . B 4
C32 C 0.5367(4) 0.6244(3) 0.8127(3) 0.0365(11) Uani 1 1 d . . . B 4
C31 C 0.2601(4) 0.5978(3) 0.8885(3) 0.0473(12) Uani 1 1 d . . . B 4
C15 C 0.2983(3) 0.2743(3) 0.8727(4) 0.0447(11) Uani 1 1 d . . . B 4
C20 C 0.3273(3) 0.2917(3) 0.9404(3) 0.0451(11) Uani 1 1 d . . . B 4
C65 C 0.2179(3) -0.0859(2) 0.4740(3) 0.0363(10) Uani 1 1 d . . . A 4
C59 C 0.4046(4) -0.0630(3) 0.4229(3) 0.0453(11) Uani 1 1 d . . . A 4
C30 C 0.1504(3) 0.6030(3) 0.9564(3) 0.0450(11) Uani 1 1 d . . . B 4
C24 C 0.3226(4) 0.5804(3) 1.0107(3) 0.0457(12) Uani 1 1 d . . . B 4
C61 C 0.5392(4) -0.1084(3) 0.2843(4) 0.0666(14) Uani 1 1 d . . . A 4
H61 H 0.6104 -0.1129 0.2436 0.080 Uiso 1 1 calc R U . A 4
C29 C 0.0618(4) 0.6148(3) 0.9336(3) 0.0621(13) Uani 1 1 d . . . B 4
H29 H 0.0706 0.6216 0.8717 0.075 Uiso 1 1 calc R U . B 4
C36 C 0.5702(5) 0.8989(3) 0.7972(4) 0.0685(14) Uani 1 1 d . . . B 4
H36 H 0.5766 0.9594 0.7923 0.082 Uiso 1 1 calc R U . B 4
C69 C 0.1241(4) -0.3466(4) 0.6613(3) 0.0683(14) Uani 1 1 d . . . A 4
H69 H 0.1896 -0.3793 0.6413 0.082 Uiso 1 1 calc R U . A 4
C27 C -0.0514(4) 0.6062(3) 1.0944(4) 0.0749(15) Uani 1 1 d . . . B 4
H27 H -0.1198 0.6061 1.1408 0.090 Uiso 1 1 calc R U . B 4
C37 C 0.6527(4) 0.8455(4) 0.7443(3) 0.0667(14) Uani 1 1 d . . . B 4
H37 H 0.7163 0.8696 0.7039 0.080 Uiso 1 1 calc R U . B 4
C40 C -0.3377(4) 0.0850(4) 0.8946(3) 0.0732(15) Uani 1 1 d . . . A 4
H40 H -0.3993 0.0575 0.9341 0.088 Uiso 1 1 calc R U . A 4
C28 C -0.0383(4) 0.6164(3) 1.0027(5) 0.0736(15) Uani 1 1 d . . . B 4
H28 H -0.0978 0.6243 0.9878 0.088 Uiso 1 1 calc R U . B 4
C7 C 0.8665(4) 0.3434(3) 0.5845(3) 0.0644(14) Uani 1 1 d . . . B 4
H7 H 0.9251 0.3121 0.5444 0.077 Uiso 1 1 calc R U . B 4
C70 C 0.0320(6) -0.3886(3) 0.6953(4) 0.0729(15) Uani 1 1 d . . . A 4
H70 H 0.0347 -0.4499 0.6974 0.087 Uiso 1 1 calc R U . A 4
O1 O 0.6277(2) 0.57901(19) 0.75817(17) 0.0393(7) Uani 1 1 d . . . B 4
O2 O 0.3892(3) 0.5707(2) 1.0437(2) 0.0697(10) Uani 1 1 d . . . B 4
O3 O 0.2188(3) 0.58422(19) 1.07486(18) 0.0573(8) Uani 1 1 d . . . B 4
O4 O 0.2681(2) 0.6035(2) 0.8014(2) 0.0759(10) Uani 1 1 d . . . B 4
H4 H 0.3312 0.5989 0.7662 0.114 Uiso 1 1 calc R U . B 4
O5 O 0.4187(2) 0.4327(2) 0.6873(2) 0.0713(10) Uani 1 1 d . . . B 4
O6 O 0.3328(2) 0.3224(2) 0.7863(2) 0.0537(8) Uani 1 1 d . . . B 4
O7 O 0.4255(2) 0.37231(19) 0.9864(2) 0.0665(9) Uani 1 1 d . . . B 4
H7A H 0.4643 0.4135 0.9703 0.100 Uiso 1 1 calc R U . B 4
O8 O 0.3806(2) -0.02447(19) 0.5018(2) 0.0573(8) Uani 1 1 d . . . A 4
O9 O 0.2693(2) 0.0070(2) 0.6405(2) 0.0648(9) Uani 1 1 d . . . A 4
O10 O 0.1464(2) -0.11315(17) 0.44910(17) 0.0479(8) Uani 1 1 d . . . A 4
H10 H 0.0869 -0.1077 0.4905 0.072 Uiso 1 1 calc R U . A 4
O11 O -0.0744(2) -0.06914(19) 0.73811(16) 0.0373(7) Uani 1 1 d . . . A 4
O12 O 0.0709(2) 0.11254(18) 0.47334(19) 0.0458(8) Uani 1 1 d . . . A 4
O13 O 0.1343(2) 0.2339(2) 0.48067(17) 0.0447(7) Uani 1 1 d . . . A 4
O14 O 0.1090(2) 0.15143(17) 0.7474(2) 0.0540(8) Uani 1 1 d . . . A 4
H14 H 0.0832 0.1033 0.7684 0.081 Uiso 1 1 calc R U . A 4
C2 C 0.1943(6) 0.8475(4) 0.8153(4) 0.137(3) Uani 1 1 d D . . C 4
H2A H 0.2028 0.8619 0.7516 0.205 Uiso 1 1 calc R U . C 4
H2B H 0.1790 0.7864 0.8354 0.205 Uiso 1 1 calc R U . C 4
H2C H 0.2589 0.8570 0.8208 0.205 Uiso 1 1 calc R U . C 4
C1 C 0.1200(5) 0.8914(4) 0.9844(3) 0.130(3) Uani 1 1 d D . . C 4
H1A H 0.1952 0.8859 0.9695 0.195 Uiso 1 1 calc R U . C 4
H1B H 0.0891 0.8379 1.0207 0.195 Uiso 1 1 calc R U . C 4
H1C H 0.0876 0.9406 1.0194 0.195 Uiso 1 1 calc R U . C 4
O15 O 0.0780(3) 0.9978(2) 0.8561(2) 0.0915(11) Uani 1 1 d . . . C 4
S2 S 0.4383(6) 0.7358(6) 0.5874(5) 0.116(4) Uani 0.282(6) 1 d D U P D 1
C3 C 0.526(2) 0.8077(19) 0.581(2) 0.092(9) Uani 0.282(6) 1 d D U P D 1
H3A H 0.5073 0.8252 0.6410 0.138 Uiso 0.282(6) 1 calc R U P D 1
H3B H 0.5230 0.8591 0.5380 0.138 Uiso 0.282(6) 1 calc R U P D 1
H3C H 0.5966 0.7793 0.5593 0.138 Uiso 0.282(6) 1 calc R U P D 1
C4 C 0.493(2) 0.7013(17) 0.4832(11) 0.098(8) Uani 0.282(6) 1 d D U P D 1
H4A H 0.5625 0.7228 0.4500 0.147 Uiso 0.282(6) 1 calc R U P D 1
H4B H 0.4489 0.7234 0.4494 0.147 Uiso 0.282(6) 1 calc R U P D 1
H4C H 0.4984 0.6376 0.4900 0.147 Uiso 0.282(6) 1 calc R U P D 1
O16 O 0.440(3) 0.6671(19) 0.6623(19) 0.128(9) Uani 0.282(6) 1 d D U P D 1
S2' S 0.5044(2) 0.6763(2) 0.5997(2) 0.1020(13) Uani 0.718(6) 1 d D U P D 2
C3' C 0.5581(11) 0.7760(10) 0.5442(11) 0.183(9) Uani 0.718(6) 1 d D U P D 2
H3'1 H 0.5038 0.8172 0.5342 0.275 Uiso 0.718(6) 1 calc R U P D 2
H3'2 H 0.6150 0.7667 0.4855 0.275 Uiso 0.718(6) 1 calc R U P D 2
H3'3 H 0.5852 0.7995 0.5821 0.275 Uiso 0.718(6) 1 calc R U P D 2
C4' C 0.4785(13) 0.6380(11) 0.5177(9) 0.203(7) Uani 0.718(6) 1 d D U P D 2
H4'1 H 0.4790 0.5744 0.5290 0.304 Uiso 0.718(6) 1 calc R U P D 2
H4'2 H 0.5320 0.6553 0.4574 0.304 Uiso 0.718(6) 1 calc R U P D 2
H4'3 H 0.4097 0.6624 0.5200 0.304 Uiso 0.718(6) 1 calc R U P D 2
O16' O 0.3926(7) 0.6962(7) 0.6727(6) 0.100(3) Uani 0.718(6) 1 d D U P D 2
S1 S 0.1703(3) 0.94341(15) 0.86782(12) 0.0707(12) Uani 0.791(8) 1 d D U P E 3
S1' S 0.0973(12) 0.9097(9) 0.8791(6) 0.109(5) Uani 0.209(8) 1 d D U P C 4


_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
C57 C65 1.348(5) . ?
C57 C58 1.436(5) . ?
C57 C56 1.480(5) . ?
C56 C66 1.361(5) . ?
C56 C46 1.428(5) . ?
C64 C59 1.377(5) . ?
C64 C63 1.401(5) . ?
C64 C65 1.445(5) . ?
C47 C55 1.360(5) . ?
C47 C48 1.439(5) . ?
C47 C46 1.472(5) . ?
C45 C46 1.354(5) . ?
C45 O11 1.380(4) . ?
C45 C44 1.464(5) . ?
C13 C21 1.346(5) . ?
C13 C14 1.445(5) . ?
C13 C12 1.482(5) . ?
C11 C12 1.357(5) . ?
C11 O1 1.372(4) . ?
C11 C10 1.454(5) . ?
C66 O11 1.377(4) . ?
C66 C67 1.463(5) . ?
C54 C49 1.379(5) . ?
C54 C53 1.390(5) . ?
C54 C55 1.439(5) . ?
C67 C72 1.375(5) . ?
C67 C68 1.385(5) . ?
C23 C31 1.347(5) . ?
C23 C24 1.433(5) . ?
C23 C22 1.479(5) . ?
C48 O12 1.210(4) . ?
C48 O13 1.378(4) . ?
C49 O13 1.377(4) . ?
C49 C50 1.382(5) . ?
C10 C9 1.381(5) . ?
C10 C5 1.381(5) . ?
C55 O14 1.330(4) . ?
C12 C22 1.446(5) . ?
C44 C43 1.383(5) . ?
C44 C39 1.389(5) . ?
C14 O5 1.204(5) . ?
C14 O6 1.393(5) . ?
C58 O9 1.210(4) . ?
C58 O8 1.381(5) . ?
C9 C8 1.386(6) . ?
C9 H9 0.9300 . ?
C21 O7 1.328(4) . ?
C21 C20 1.457(5) . ?
C5 C6 1.383(5) . ?
C5 H5 0.9300 . ?
C25 C30 1.365(5) . ?
C25 O3 1.374(5) . ?
C25 C26 1.381(6) . ?
C68 C69 1.382(6) . ?
C68 H68 0.9300 . ?
C50 C51 1.367(6) . ?
C50 H50 0.9300 . ?
C63 C62 1.372(5) . ?
C63 H63 0.9300 . ?
C43 C42 1.378(5) . ?
C43 H43 0.9300 . ?
C53 C52 1.363(6) . ?
C53 H53 0.9300 . ?
C8 C7 1.364(6) . ?
C8 H8 0.9300 . ?
C16 C17 1.348(6) . ?
C16 C15 1.382(6) . ?
C16 H16 0.9300 . ?
C39 C40 1.381(6) . ?
C39 H39 0.9300 . ?
C60 C61 1.367(6) . ?
C60 C59 1.379(5) . ?
C60 H60 0.9300 . ?
C38 C37 1.374(6) . ?
C38 C33 1.383(5) . ?
C38 H38 0.9300 . ?
C72 C71 1.383(6) . ?
C72 H72 0.9300 . ?
C6 C7 1.376(6) . ?
C6 H6 0.9300 . ?
C42 C41 1.363(6) . ?
C42 H42 0.9300 . ?
C62 C61 1.379(6) . ?
C62 H62 0.9300 . ?
C41 C40 1.373(6) . ?
C41 H41 0.9300 . ?
C51 C52 1.373(6) . ?
C51 H51 0.9300 . ?
C52 H52 0.9300 . ?
C34 C35 1.375(6) . ?
C34 C33 1.380(5) . ?
C34 H34 0.9300 . ?
C26 C27 1.358(6) . ?
C26 H26 0.9300 . ?
C17 C18 1.377(7) . ?
C17 H17 0.9300 . ?
C35 C36 1.364(6) . ?
C35 H35 0.9300 . ?
C19 C18 1.373(6) . ?
C19 C20 1.382(6) . ?
C19 H19 0.9300 . ?
C71 C70 1.357(6) . ?
C71 H71 0.9300 . ?
C18 H18 0.9300 . ?
C22 C32 1.358(5) . ?
C33 C32 1.463(5) . ?
C32 O1 1.374(4) . ?
C31 O4 1.331(5) . ?
C31 C30 1.456(5) . ?
C15 C20 1.362(5) . ?
C15 O6 1.371(5) . ?
C65 O10 1.333(4) . ?
C59 O8 1.372(5) . ?
C30 C29 1.391(6) . ?
C24 O2 1.211(4) . ?
C24 O3 1.376(5) . ?
C61 H61 0.9300 . ?
C29 C28 1.369(6) . ?
C29 H29 0.9300 . ?
C36 C37 1.367(6) . ?
C36 H36 0.9300 . ?
C69 C70 1.361(6) . ?
C69 H69 0.9300 . ?
C27 C28 1.376(6) . ?
C27 H27 0.9300 . ?
C37 H37 0.9300 . ?
C40 H40 0.9300 . ?
C28 H28 0.9300 . ?
C7 H7 0.9300 . ?
C70 H70 0.9300 . ?
O4 H4 0.8200 . ?
O7 H7A 0.8200 . ?
O10 H10 0.8200 . ?
O14 H14 0.8200 . ?
C2 S1' 1.612(10) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C1 S1' 1.796(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
O15 S1' 1.359(11) . ?
S2 O16 1.459(19) . ?
S2 C4 1.657(16) . ?
S2 C3 1.698(17) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
S2' O16' 1.531(8) . ?
S2' C4' 1.689(13) . ?
S2' C3' 1.726(13) . ?
C3' H3'1 0.9600 . ?
C3' H3'2 0.9600 . ?
C3' H3'3 0.9600 . ?
C4' H4'1 0.9600 . ?
C4' H4'2 0.9600 . ?
C4' H4'3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C65 C57 C58 119.7(4) . . ?
C65 C57 C56 123.7(4) . . ?
C58 C57 C56 116.4(4) . . ?
C66 C56 C46 107.1(3) . . ?
C66 C56 C57 129.2(4) . . ?
C46 C56 C57 123.7(4) . . ?
C59 C64 C63 117.2(4) . . ?
C59 C64 C65 117.7(4) . . ?
C63 C64 C65 125.1(4) . . ?
C55 C47 C48 120.1(4) . . ?
C55 C47 C46 123.4(4) . . ?
C48 C47 C46 116.3(4) . . ?
C46 C45 O11 109.2(3) . . ?
C46 C45 C44 135.9(4) . . ?
O11 C45 C44 114.9(4) . . ?
C21 C13 C14 119.7(4) . . ?
C21 C13 C12 122.0(4) . . ?
C14 C13 C12 117.9(4) . . ?
C45 C46 C56 107.1(3) . . ?
C45 C46 C47 128.5(4) . . ?
C56 C46 C47 124.4(4) . . ?
C12 C11 O1 109.1(3) . . ?
C12 C11 C10 136.2(4) . . ?
O1 C11 C10 114.7(4) . . ?
C56 C66 O11 108.9(3) . . ?
C56 C66 C67 135.3(4) . . ?
O11 C66 C67 115.7(4) . . ?
C49 C54 C53 117.6(4) . . ?
C49 C54 C55 118.4(4) . . ?
C53 C54 C55 124.0(4) . . ?
C72 C67 C68 117.7(4) . . ?
C72 C67 C66 121.2(4) . . ?
C68 C67 C66 121.1(4) . . ?
C31 C23 C24 118.6(4) . . ?
C31 C23 C22 123.1(4) . . ?
C24 C23 C22 117.8(4) . . ?
O12 C48 O13 115.8(4) . . ?
O12 C48 C47 125.9(4) . . ?
O13 C48 C47 118.3(4) . . ?
O13 C49 C54 121.1(4) . . ?
O13 C49 C50 116.7(4) . . ?
C54 C49 C50 122.2(4) . . ?
C9 C10 C5 118.2(4) . . ?
C9 C10 C11 121.9(4) . . ?
C5 C10 C11 119.8(4) . . ?
O14 C55 C47 124.8(4) . . ?
O14 C55 C54 115.0(4) . . ?
C47 C55 C54 120.2(4) . . ?
C11 C12 C22 106.9(3) . . ?
C11 C12 C13 129.4(4) . . ?
C22 C12 C13 123.6(4) . . ?
C43 C44 C39 116.6(4) . . ?
C43 C44 C45 122.1(4) . . ?
C39 C44 C45 121.4(4) . . ?
O5 C14 O6 116.0(4) . . ?
O5 C14 C13 126.3(4) . . ?
O6 C14 C13 117.6(4) . . ?
O9 C58 O8 115.9(4) . . ?
O9 C58 C57 125.9(4) . . ?
O8 C58 C57 118.2(4) . . ?
C10 C9 C8 120.8(4) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
O7 C21 C13 125.1(4) . . ?
O7 C21 C20 113.5(4) . . ?
C13 C21 C20 121.3(4) . . ?
C10 C5 C6 121.1(4) . . ?
C10 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C30 C25 O3 121.4(4) . . ?
C30 C25 C26 122.2(4) . . ?
O3 C25 C26 116.4(5) . . ?
C69 C68 C67 121.1(4) . . ?
C69 C68 H68 119.5 . . ?
C67 C68 H68 119.5 . . ?
C51 C50 C49 118.4(4) . . ?
C51 C50 H50 120.8 . . ?
C49 C50 H50 120.8 . . ?
C62 C63 C64 120.9(4) . . ?
C62 C63 H63 119.5 . . ?
C64 C63 H63 119.5 . . ?
C42 C43 C44 122.3(4) . . ?
C42 C43 H43 118.9 . . ?
C44 C43 H43 118.9 . . ?
C52 C53 C54 120.8(4) . . ?
C52 C53 H53 119.6 . . ?
C54 C53 H53 119.6 . . ?
C7 C8 C9 120.1(4) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C17 C16 C15 118.9(5) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C40 C39 C44 121.0(4) . . ?
C40 C39 H39 119.5 . . ?
C44 C39 H39 119.5 . . ?
C61 C60 C59 118.9(4) . . ?
C61 C60 H60 120.6 . . ?
C59 C60 H60 120.6 . . ?
C37 C38 C33 121.2(4) . . ?
C37 C38 H38 119.4 . . ?
C33 C38 H38 119.4 . . ?
C67 C72 C71 121.0(4) . . ?
C67 C72 H72 119.5 . . ?
C71 C72 H72 119.5 . . ?
C7 C6 C5 119.6(4) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C41 C42 C43 120.3(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C63 C62 C61 119.9(4) . . ?
C63 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C42 C41 C40 118.8(4) . . ?
C42 C41 H41 120.6 . . ?
C40 C41 H41 120.6 . . ?
C50 C51 C52 120.8(4) . . ?
C50 C51 H51 119.6 . . ?
C52 C51 H51 119.6 . . ?
C53 C52 C51 120.3(4) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C35 C34 C33 120.6(4) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C27 C26 C25 118.1(5) . . ?
C27 C26 H26 121.0 . . ?
C25 C26 H26 121.0 . . ?
C16 C17 C18 120.2(5) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C36 C35 C34 121.2(5) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C18 C19 C20 119.7(5) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C70 C71 C72 120.2(5) . . ?
C70 C71 H71 119.9 . . ?
C72 C71 H71 119.9 . . ?
C19 C18 C17 120.5(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C32 C22 C12 106.4(3) . . ?
C32 C22 C23 129.8(4) . . ?
C12 C22 C23 123.9(4) . . ?
C34 C33 C38 117.7(4) . . ?
C34 C33 C32 121.4(4) . . ?
C38 C33 C32 120.9(4) . . ?
C22 C32 O1 109.3(3) . . ?
C22 C32 C33 136.6(4) . . ?
O1 C32 C33 113.7(4) . . ?
O4 C31 C23 124.8(4) . . ?
O4 C31 C30 113.4(4) . . ?
C23 C31 C30 121.8(4) . . ?
C20 C15 O6 121.6(4) . . ?
C20 C15 C16 122.2(4) . . ?
O6 C15 C16 116.1(5) . . ?
C15 C20 C19 118.3(4) . . ?
C15 C20 C21 117.7(4) . . ?
C19 C20 C21 124.0(5) . . ?
O10 C65 C57 125.2(4) . . ?
O10 C65 C64 113.6(4) . . ?
C57 C65 C64 121.2(4) . . ?
O8 C59 C64 121.0(4) . . ?
O8 C59 C60 116.5(4) . . ?
C64 C59 C60 122.5(4) . . ?
C25 C30 C29 118.6(4) . . ?
C25 C30 C31 117.4(4) . . ?
C29 C30 C31 123.9(5) . . ?
O2 C24 O3 114.6(4) . . ?
O2 C24 C23 126.0(4) . . ?
O3 C24 C23 119.4(4) . . ?
C60 C61 C62 120.6(4) . . ?
C60 C61 H61 119.7 . . ?
C62 C61 H61 119.7 . . ?
C28 C29 C30 119.6(4) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C35 C36 C37 118.8(5) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C70 C69 C68 119.9(5) . . ?
C70 C69 H69 120.1 . . ?
C68 C69 H69 120.1 . . ?
C26 C27 C28 121.2(5) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C36 C37 C38 120.5(4) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C41 C40 C39 121.0(4) . . ?
C41 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C29 C28 C27 120.2(5) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C8 C7 C6 120.1(4) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C71 C70 C69 120.1(5) . . ?
C71 C70 H70 119.9 . . ?
C69 C70 H70 119.9 . . ?
C11 O1 C32 108.2(3) . . ?
C25 O3 C24 121.3(4) . . ?
C31 O4 H4 109.5 . . ?
C15 O6 C14 121.8(4) . . ?
C21 O7 H7A 109.5 . . ?
C59 O8 C58 121.7(3) . . ?
C65 O10 H10 109.5 . . ?
C66 O11 C45 107.7(3) . . ?
C49 O13 C48 121.4(3) . . ?
C55 O14 H14 109.5 . . ?
S1' C2 H2A 109.5 . . ?
S1' C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S1' C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
S1' C1 H1A 109.5 . . ?
S1' C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S1' C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O16 S2 C4 113.6(17) . . ?
O16 S2 C3 104(2) . . ?
C4 S2 C3 102.6(15) . . ?
S2 C3 H3A 109.5 . . ?
S2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
S2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S2 C4 H4A 109.5 . . ?
S2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
S2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O16' S2' C4' 102.6(8) . . ?
O16' S2' C3' 108.2(6) . . ?
C4' S2' C3' 102.8(8) . . ?
S2' C3' H3'1 109.5 . . ?
S2' C3' H3'2 109.5 . . ?
H3'1 C3' H3'2 109.5 . . ?
S2' C3' H3'3 109.5 . . ?
H3'1 C3' H3'3 109.5 . . ?
H3'2 C3' H3'3 109.5 . . ?
S2' C4' H4'1 109.5 . . ?
S2' C4' H4'2 109.5 . . ?
H4'1 C4' H4'2 109.5 . . ?
S2' C4' H4'3 109.5 . . ?
H4'1 C4' H4'3 109.5 . . ?
H4'2 C4' H4'3 109.5 . . ?
O15 S1' C2 125.0(10) . . ?
O15 S1' C1 110.3(8) . . ?
C2 S1' C1 100.5(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C65 C57 C56 C66 63.0(6) . . . . ?
C58 C57 C56 C66 -120.7(4) . . . . ?
C65 C57 C56 C46 -117.7(4) . . . . ?
C58 C57 C56 C46 58.6(5) . . . . ?
O11 C45 C46 C56 0.1(4) . . . . ?
C44 C45 C46 C56 -178.5(4) . . . . ?
O11 C45 C46 C47 176.7(3) . . . . ?
C44 C45 C46 C47 -1.8(7) . . . . ?
C66 C56 C46 C45 -0.8(4) . . . . ?
C57 C56 C46 C45 179.8(3) . . . . ?
C66 C56 C46 C47 -177.6(3) . . . . ?
C57 C56 C46 C47 3.0(5) . . . . ?
C55 C47 C46 C45 74.1(5) . . . . ?
C48 C47 C46 C45 -109.8(4) . . . . ?
C55 C47 C46 C56 -109.8(4) . . . . ?
C48 C47 C46 C56 66.3(5) . . . . ?
C46 C56 C66 O11 1.1(4) . . . . ?
C57 C56 C66 O11 -179.5(3) . . . . ?
C46 C56 C66 C67 -178.5(4) . . . . ?
C57 C56 C66 C67 0.9(7) . . . . ?
C56 C66 C67 C72 -158.2(4) . . . . ?
O11 C66 C67 C72 22.2(5) . . . . ?
C56 C66 C67 C68 22.6(6) . . . . ?
O11 C66 C67 C68 -157.0(3) . . . . ?
C55 C47 C48 O12 175.9(4) . . . . ?
C46 C47 C48 O12 -0.4(5) . . . . ?
C55 C47 C48 O13 -3.7(5) . . . . ?
C46 C47 C48 O13 -180.0(3) . . . . ?
C53 C54 C49 O13 178.6(3) . . . . ?
C55 C54 C49 O13 -2.6(5) . . . . ?
C53 C54 C49 C50 -1.0(6) . . . . ?
C55 C54 C49 C50 177.7(4) . . . . ?
C12 C11 C10 C9 37.1(7) . . . . ?
O1 C11 C10 C9 -144.0(4) . . . . ?
C12 C11 C10 C5 -147.1(4) . . . . ?
O1 C11 C10 C5 31.8(5) . . . . ?
C48 C47 C55 O14 -176.3(3) . . . . ?
C46 C47 C55 O14 -0.3(6) . . . . ?
C48 C47 C55 C54 6.7(5) . . . . ?
C46 C47 C55 C54 -177.3(3) . . . . ?
C49 C54 C55 O14 179.1(3) . . . . ?
C53 C54 C55 O14 -2.2(5) . . . . ?
C49 C54 C55 C47 -3.6(5) . . . . ?
C53 C54 C55 C47 175.1(4) . . . . ?
O1 C11 C12 C22 -0.3(4) . . . . ?
C10 C11 C12 C22 178.7(4) . . . . ?
O1 C11 C12 C13 -179.2(3) . . . . ?
C10 C11 C12 C13 -0.3(7) . . . . ?
C21 C13 C12 C11 107.5(5) . . . . ?
C14 C13 C12 C11 -79.4(5) . . . . ?
C21 C13 C12 C22 -71.3(5) . . . . ?
C14 C13 C12 C22 101.8(4) . . . . ?
C46 C45 C44 C43 -5.6(7) . . . . ?
O11 C45 C44 C43 175.9(3) . . . . ?
C46 C45 C44 C39 174.4(4) . . . . ?
O11 C45 C44 C39 -4.1(5) . . . . ?
C21 C13 C14 O5 177.7(4) . . . . ?
C12 C13 C14 O5 4.5(6) . . . . ?
C21 C13 C14 O6 -3.6(5) . . . . ?
C12 C13 C14 O6 -176.8(3) . . . . ?
C65 C57 C58 O9 -179.7(4) . . . . ?
C56 C57 C58 O9 3.9(6) . . . . ?
C65 C57 C58 O8 0.8(6) . . . . ?
C56 C57 C58 O8 -175.7(3) . . . . ?
C5 C10 C9 C8 -1.7(6) . . . . ?
C11 C10 C9 C8 174.2(4) . . . . ?
C14 C13 C21 O7 -177.6(4) . . . . ?
C12 C13 C21 O7 -4.7(6) . . . . ?
C14 C13 C21 C20 -0.2(6) . . . . ?
C12 C13 C21 C20 172.7(4) . . . . ?
C9 C10 C5 C6 1.6(6) . . . . ?
C11 C10 C5 C6 -174.4(4) . . . . ?
C72 C67 C68 C69 1.7(6) . . . . ?
C66 C67 C68 C69 -179.2(4) . . . . ?
O13 C49 C50 C51 -179.4(4) . . . . ?
C54 C49 C50 C51 0.3(6) . . . . ?
C59 C64 C63 C62 0.3(6) . . . . ?
C65 C64 C63 C62 -178.6(4) . . . . ?
C39 C44 C43 C42 -0.4(6) . . . . ?
C45 C44 C43 C42 179.6(4) . . . . ?
C49 C54 C53 C52 0.7(6) . . . . ?
C55 C54 C53 C52 -178.0(4) . . . . ?
C10 C9 C8 C7 0.5(6) . . . . ?
C43 C44 C39 C40 -0.5(6) . . . . ?
C45 C44 C39 C40 179.6(4) . . . . ?
C68 C67 C72 C71 -1.1(6) . . . . ?
C66 C67 C72 C71 179.7(4) . . . . ?
C10 C5 C6 C7 -0.4(6) . . . . ?
C44 C43 C42 C41 0.7(6) . . . . ?
C64 C63 C62 C61 -1.3(6) . . . . ?
C43 C42 C41 C40 0.0(7) . . . . ?
C49 C50 C51 C52 0.8(7) . . . . ?
C54 C53 C52 C51 0.4(7) . . . . ?
C50 C51 C52 C53 -1.2(7) . . . . ?
C30 C25 C26 C27 0.2(7) . . . . ?
O3 C25 C26 C27 -179.6(4) . . . . ?
C15 C16 C17 C18 0.8(7) . . . . ?
C33 C34 C35 C36 -0.3(7) . . . . ?
C67 C72 C71 C70 -0.6(7) . . . . ?
C20 C19 C18 C17 2.8(8) . . . . ?
C16 C17 C18 C19 -3.1(8) . . . . ?
C11 C12 C22 C32 1.3(4) . . . . ?
C13 C12 C22 C32 -179.7(4) . . . . ?
C11 C12 C22 C23 -177.4(4) . . . . ?
C13 C12 C22 C23 1.6(6) . . . . ?
C31 C23 C22 C32 108.7(5) . . . . ?
C24 C23 C22 C32 -79.2(5) . . . . ?
C31 C23 C22 C12 -72.9(5) . . . . ?
C24 C23 C22 C12 99.2(4) . . . . ?
C35 C34 C33 C38 1.0(6) . . . . ?
C35 C34 C33 C32 -176.1(4) . . . . ?
C37 C38 C33 C34 -0.7(6) . . . . ?
C37 C38 C33 C32 176.4(4) . . . . ?
C12 C22 C32 O1 -1.8(4) . . . . ?
C23 C22 C32 O1 176.8(4) . . . . ?
C12 C22 C32 C33 170.8(4) . . . . ?
C23 C22 C32 C33 -10.6(7) . . . . ?
C34 C33 C32 C22 10.8(7) . . . . ?
C38 C33 C32 C22 -166.2(4) . . . . ?
C34 C33 C32 O1 -176.9(3) . . . . ?
C38 C33 C32 O1 6.1(5) . . . . ?
C24 C23 C31 O4 -178.9(4) . . . . ?
C22 C23 C31 O4 -6.8(6) . . . . ?
C24 C23 C31 C30 0.1(6) . . . . ?
C22 C23 C31 C30 172.1(4) . . . . ?
C17 C16 C15 C20 1.8(6) . . . . ?
C17 C16 C15 O6 -176.4(4) . . . . ?
O6 C15 C20 C19 176.0(4) . . . . ?
C16 C15 C20 C19 -2.2(6) . . . . ?
O6 C15 C20 C21 -2.6(6) . . . . ?
C16 C15 C20 C21 179.2(4) . . . . ?
C18 C19 C20 C15 -0.1(7) . . . . ?
C18 C19 C20 C21 178.4(4) . . . . ?
O7 C21 C20 C15 -179.0(3) . . . . ?
C13 C21 C20 C15 3.3(6) . . . . ?
O7 C21 C20 C19 2.5(6) . . . . ?
C13 C21 C20 C19 -175.2(4) . . . . ?
C58 C57 C65 O10 -176.5(3) . . . . ?
C56 C57 C65 O10 -0.3(6) . . . . ?
C58 C57 C65 C64 5.0(6) . . . . ?
C56 C57 C65 C64 -178.9(3) . . . . ?
C59 C64 C65 O10 175.6(3) . . . . ?
C63 C64 C65 O10 -5.5(5) . . . . ?
C59 C64 C65 C57 -5.7(5) . . . . ?
C63 C64 C65 C57 173.2(4) . . . . ?
C63 C64 C59 O8 -178.4(3) . . . . ?
C65 C64 C59 O8 0.6(6) . . . . ?
C63 C64 C59 C60 1.4(6) . . . . ?
C65 C64 C59 C60 -179.6(4) . . . . ?
C61 C60 C59 O8 177.7(4) . . . . ?
C61 C60 C59 C64 -2.1(7) . . . . ?
O3 C25 C30 C29 -179.1(4) . . . . ?
C26 C25 C30 C29 1.1(6) . . . . ?
O3 C25 C30 C31 1.5(6) . . . . ?
C26 C25 C30 C31 -178.3(4) . . . . ?
O4 C31 C30 C25 177.9(4) . . . . ?
C23 C31 C30 C25 -1.2(6) . . . . ?
O4 C31 C30 C29 -1.4(6) . . . . ?
C23 C31 C30 C29 179.5(4) . . . . ?
C31 C23 C24 O2 -180.0(4) . . . . ?
C22 C23 C24 O2 7.5(6) . . . . ?
C31 C23 C24 O3 0.7(5) . . . . ?
C22 C23 C24 O3 -171.8(3) . . . . ?
C59 C60 C61 C62 1.1(7) . . . . ?
C63 C62 C61 C60 0.6(7) . . . . ?
C25 C30 C29 C28 -1.2(6) . . . . ?
C31 C30 C29 C28 178.2(4) . . . . ?
C34 C35 C36 C37 -0.8(7) . . . . ?
C67 C68 C69 C70 -0.5(7) . . . . ?
C25 C26 C27 C28 -1.5(7) . . . . ?
C35 C36 C37 C38 1.2(7) . . . . ?
C33 C38 C37 C36 -0.4(7) . . . . ?
C42 C41 C40 C39 -0.8(7) . . . . ?
C44 C39 C40 C41 1.1(7) . . . . ?
C30 C29 C28 C27 0.0(7) . . . . ?
C26 C27 C28 C29 1.4(8) . . . . ?
C9 C8 C7 C6 0.9(7) . . . . ?
C5 C6 C7 C8 -0.9(7) . . . . ?
C72 C71 C70 C69 1.8(8) . . . . ?
C68 C69 C70 C71 -1.3(7) . . . . ?
C12 C11 O1 C32 -0.8(4) . . . . ?
C10 C11 O1 C32 180.0(3) . . . . ?
C22 C32 O1 C11 1.7(4) . . . . ?
C33 C32 O1 C11 -172.8(3) . . . . ?
C30 C25 O3 C24 -0.7(6) . . . . ?
C26 C25 O3 C24 179.1(4) . . . . ?
O2 C24 O3 C25 -179.8(4) . . . . ?
C23 C24 O3 C25 -0.5(5) . . . . ?
C20 C15 O6 C14 -1.4(5) . . . . ?
C16 C15 O6 C14 177.0(3) . . . . ?
O5 C14 O6 C15 -176.7(4) . . . . ?
C13 C14 O6 C15 4.5(5) . . . . ?
C64 C59 O8 C58 5.3(6) . . . . ?
C60 C59 O8 C58 -174.6(4) . . . . ?
O9 C58 O8 C59 174.5(4) . . . . ?
C57 C58 O8 C59 -6.0(5) . . . . ?
C56 C66 O11 C45 -1.1(4) . . . . ?
C67 C66 O11 C45 178.6(3) . . . . ?
C46 C45 O11 C66 0.6(4) . . . . ?
C44 C45 O11 C66 179.5(3) . . . . ?
C54 C49 O13 C48 5.6(5) . . . . ?
C50 C49 O13 C48 -174.7(3) . . . . ?
O12 C48 O13 C49 177.9(3) . . . . ?
C47 C48 O13 C49 -2.5(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
O10 H10 O12 0.82 2.02 2.731(4) 145.5 2_556
O7 H7A O2 0.82 1.98 2.638(4) 136.5 2_667
C60 H60 O9 0.93 2.38 3.270(5) 159.9 2_656
C16 H16 O14 0.93 2.66 3.553(5) 162.2 .

_refine_diff_density_max         0.233
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.033

# start Validation Reply Form
_vrf_THETM01_asim                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal quality is poor and higher angle reflections
are very weak. The reflections above 19 degrees are omitted from
refinement for better R factor
;
_vrf_PLAT023_asim                
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      18.87 Degree
RESPONSE: The size of crystals are very small and weakly scattering, No data 
were detected beyond that collected.
;
_vrf_PLAT088_asim                
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.48 Note  
RESPONSE: The crystal quality is poor and higher angle reflections are
very weak. The reflections above 19 degrees are omitted from refinement.
This caused poor data/parameter ratio
;
_vrf_PLAT212_asim                
;
PROBLEM: ADP of Atom C4        is N.P.D. or (nearly) 2D .     Please Check 
RESPONSE: Some disordered atoms refined to small displacement parameters
;
_vrf_PLAT306_asim                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O15 Check 
RESPONSE: Hydrogen atoms of the disordered solvate  molecules were
not located.
;
# end Validation Reply Form

