# Supplementary Information (SI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2025

####################################################################### 
# 
# 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_2_wa3589-DESY-P24
_database_code_depnum_ccdc_archive 'CCDC 2384683'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT911_2_wa3589-DESY-P24   
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600          9 Report
RESPONSE: These reflections are hidden by the beamstop or located
in the Lorentz area of the detector.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H28 B2 O2 S4'
_chemical_formula_sum            'C36 H28 B2 O2 S4'
_chemical_formula_weight         642.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0013 0.0009 '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'
B B 0.0007 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0058 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.0831 0.0770 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   20.9778(6)
_cell_length_b                   20.7457(5)
_cell_length_c                   7.3237(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.674(3)
_cell_angle_gamma                90
_cell_volume                     3150.80(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    4266
_cell_measurement_theta_min      1.5400
_cell_measurement_theta_max      27.4560

_exptl_crystal_description       needle
_exptl_crystal_colour            'pale brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.176
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_T_min  0.08103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.126a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.560
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device       
'DESY Petra3 P24 beamline, Huber diffractometer, Lambda 7.5M CdTe'
_diffrn_detector_area_resol_mean 18.2
_diffrn_measurement_method       'φ scans'
_diffrn_detector                 
'X-Spectrum Lambda 7.5M CdTe photon-counting detector'
_diffrn_reflns_number            19919
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.547
_diffrn_reflns_theta_max         20.482
_diffrn_reflns_theta_full        19.633
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3224
_reflns_number_gt                2501
_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       'P24 beamline local software'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_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)+(0.0526P)²+1.7224P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         3224
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1098
_refine_ls_wR_factor_gt          0.1041
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.35770(3) 0.50360(2) 0.31478(7) 0.02615(15) Uani 1 1 d . . . . .
S2 S 0.36946(3) 0.77558(3) -0.00406(8) 0.03429(17) Uani 1 1 d . . . . .
B1 B 0.30099(12) 0.63077(12) 0.2592(3) 0.0281(5) Uani 1 1 d . . . . .
O1 O 0.30937(7) 0.69153(7) 0.1854(2) 0.0307(3) Uani 1 1 d . . . . .
C1 C 0.46921(10) 0.43641(10) 0.2698(3) 0.0262(4) Uani 1 1 d . . . . .
H1 H 0.448257 0.396941 0.289079 0.031 Uiso 1 1 calc R U . . .
C2 C 0.43701(10) 0.49571(9) 0.2817(3) 0.0237(4) Uani 1 1 d . . . . .
C3 C 0.46608(10) 0.55557(9) 0.2528(2) 0.0232(4) Uani 1 1 d . . . . .
C4 C 0.41764(10) 0.60542(10) 0.2250(3) 0.0247(4) Uani 1 1 d . . . . .
C5 C 0.35814(10) 0.58501(10) 0.2651(3) 0.0258(4) Uani 1 1 d . . . . .
C6 C 0.36502(11) 0.70594(10) 0.1218(3) 0.0280(5) Uani 1 1 d . . . . .
C7 C 0.41954(10) 0.66842(9) 0.1375(3) 0.0254(4) Uani 1 1 d . . . . .
C8 C 0.46653(11) 0.69835(10) 0.0416(3) 0.0277(5) Uani 1 1 d . . . . .
H8 H 0.507764 0.680297 0.035376 0.033 Uiso 1 1 calc R U . . .
C9 C 0.44616(11) 0.75494(11) -0.0392(3) 0.0326(5) Uani 1 1 d . . . . .
H9 H 0.471563 0.780581 -0.108054 0.039 Uiso 1 1 calc R U . . .
C10 C 0.23568(10) 0.61829(10) 0.3311(3) 0.0269(4) Uani 1 1 d . . . . .
C11 C 0.18491(11) 0.58537(10) 0.2215(3) 0.0311(5) Uani 1 1 d . . . . .
C12 C 0.12627(11) 0.57828(11) 0.2852(3) 0.0381(6) Uani 1 1 d . . . . .
H12 H 0.092177 0.556451 0.209756 0.046 Uiso 1 1 calc R U . . .
C13 C 0.11576(11) 0.60197(12) 0.4549(4) 0.0407(6) Uani 1 1 d . . . . .
C14 C 0.16644(12) 0.63376(12) 0.5630(3) 0.0385(6) Uani 1 1 d . . . . .
H14 H 0.160148 0.650386 0.679834 0.046 Uiso 1 1 calc R U . . .
C15 C 0.22583(11) 0.64181(11) 0.5049(3) 0.0313(5) Uani 1 1 d . . . . .
C16 C 0.19467(13) 0.55749(12) 0.0378(3) 0.0425(6) Uani 1 1 d . . . . .
H16A H 0.224426 0.584914 -0.018431 0.064 Uiso 1 1 calc R U . . .
H16B H 0.153147 0.555416 -0.043795 0.064 Uiso 1 1 calc R U . . .
H16C H 0.212771 0.514013 0.056048 0.064 Uiso 1 1 calc R U . . .
C17 C 0.05241(13) 0.59221(15) 0.5265(5) 0.0629(9) Uani 1 1 d . . . . .
H17A H 0.045040 0.628274 0.607181 0.094 Uiso 1 1 calc R U . . .
H17B H 0.053978 0.551827 0.596421 0.094 Uiso 1 1 calc R U . . .
H17C H 0.017215 0.590226 0.422172 0.094 Uiso 1 1 calc R U . . .
C18 C 0.27993(12) 0.67521(13) 0.6303(3) 0.0431(6) Uani 1 1 d . . . . .
H18A H 0.312328 0.643326 0.680813 0.065 Uiso 1 1 calc R U . . .
H18B H 0.262496 0.696378 0.731777 0.065 Uiso 1 1 calc R U . . .
H18C H 0.299936 0.707525 0.559501 0.065 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C2 1.725(2) . ?
S1 C5 1.728(2) . ?
S2 C9 1.721(2) . ?
S2 C6 1.724(2) . ?
B1 O1 1.393(3) . ?
B1 C5 1.525(3) . ?
B1 C10 1.562(3) . ?
O1 C6 1.354(3) . ?
C1 C1 1.366(4) 2_655 ?
C1 C2 1.413(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.413(3) . ?
C3 C3 1.430(4) 2_655 ?
C3 C4 1.443(3) . ?
C4 C5 1.391(3) . ?
C4 C7 1.459(3) . ?
C6 C7 1.374(3) . ?
C7 C8 1.435(3) . ?
C8 C9 1.354(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.407(3) . ?
C10 C11 1.410(3) . ?
C11 C12 1.387(3) . ?
C11 C16 1.507(3) . ?
C12 C13 1.385(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(4) . ?
C13 C17 1.514(3) . ?
C14 C15 1.386(3) . ?
C14 H14 0.9500 . ?
C15 C18 1.516(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 S1 C5 91.55(10) . . ?
C9 S2 C6 89.91(10) . . ?
O1 B1 C5 115.4(2) . . ?
O1 B1 C10 116.71(19) . . ?
C5 B1 C10 127.8(2) . . ?
C6 O1 B1 119.94(17) . . ?
C1 C1 C2 119.31(12) 2_655 . ?
C1 C1 H1 120.3 2_655 . ?
C2 C1 H1 120.3 . . ?
C1 C2 C3 122.34(19) . . ?
C1 C2 S1 124.86(16) . . ?
C3 C2 S1 112.63(15) . . ?
C2 C3 C3 117.26(12) . 2_655 ?
C2 C3 C4 109.89(18) . . ?
C3 C3 C4 132.77(12) 2_655 . ?
C5 C4 C3 112.80(18) . . ?
C5 C4 C7 116.77(18) . . ?
C3 C4 C7 129.70(19) . . ?
C4 C5 B1 122.09(19) . . ?
C4 C5 S1 112.06(16) . . ?
B1 C5 S1 125.83(17) . . ?
O1 C6 C7 126.60(19) . . ?
O1 C6 S2 119.20(15) . . ?
C7 C6 S2 114.09(17) . . ?
C6 C7 C8 109.79(19) . . ?
C6 C7 C4 117.82(19) . . ?
C8 C7 C4 131.99(19) . . ?
C9 C8 C7 113.2(2) . . ?
C9 C8 H8 123.4 . . ?
C7 C8 H8 123.4 . . ?
C8 C9 S2 113.00(17) . . ?
C8 C9 H9 123.5 . . ?
S2 C9 H9 123.5 . . ?
C15 C10 C11 118.8(2) . . ?
C15 C10 B1 120.24(18) . . ?
C11 C10 B1 120.94(19) . . ?
C12 C11 C10 119.5(2) . . ?
C12 C11 C16 120.4(2) . . ?
C10 C11 C16 120.1(2) . . ?
C13 C12 C11 122.2(2) . . ?
C13 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
C12 C13 C14 117.8(2) . . ?
C12 C13 C17 122.0(2) . . ?
C14 C13 C17 120.1(3) . . ?
C15 C14 C13 121.8(2) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C14 C15 C10 119.8(2) . . ?
C14 C15 C18 119.7(2) . . ?
C10 C15 C18 120.5(2) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 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
C5 B1 O1 C6 1.2(3) . . . . ?
C10 B1 O1 C6 179.43(17) . . . . ?
C1 C1 C2 C3 0.4(3) 2_655 . . . ?
C1 C1 C2 S1 175.39(18) 2_655 . . . ?
C5 S1 C2 C1 -168.95(18) . . . . ?
C5 S1 C2 C3 6.42(15) . . . . ?
C1 C2 C3 C3 -12.2(3) . . . 2_655 ?
S1 C2 C3 C3 172.25(18) . . . 2_655 ?
C1 C2 C3 C4 164.86(17) . . . . ?
S1 C2 C3 C4 -10.6(2) . . . . ?
C2 C3 C4 C5 10.5(2) . . . . ?
C3 C3 C4 C5 -173.0(2) 2_655 . . . ?
C2 C3 C4 C7 -159.24(19) . . . . ?
C3 C3 C4 C7 17.3(4) 2_655 . . . ?
C3 C4 C5 B1 175.52(17) . . . . ?
C7 C4 C5 B1 -13.3(3) . . . . ?
C3 C4 C5 S1 -5.9(2) . . . . ?
C7 C4 C5 S1 165.28(14) . . . . ?
O1 B1 C5 C4 9.0(3) . . . . ?
C10 B1 C5 C4 -168.95(19) . . . . ?
O1 B1 C5 S1 -169.36(15) . . . . ?
C10 B1 C5 S1 12.7(3) . . . . ?
C2 S1 C5 C4 -0.22(15) . . . . ?
C2 S1 C5 B1 178.28(18) . . . . ?
B1 O1 C6 C7 -7.0(3) . . . . ?
B1 O1 C6 S2 169.00(15) . . . . ?
C9 S2 C6 O1 -176.28(17) . . . . ?
C9 S2 C6 C7 0.18(17) . . . . ?
O1 C6 C7 C8 176.03(18) . . . . ?
S2 C6 C7 C8 -0.1(2) . . . . ?
O1 C6 C7 C4 2.4(3) . . . . ?
S2 C6 C7 C4 -173.74(14) . . . . ?
C5 C4 C7 C6 7.7(3) . . . . ?
C3 C4 C7 C6 177.17(19) . . . . ?
C5 C4 C7 C8 -164.2(2) . . . . ?
C3 C4 C7 C8 5.3(4) . . . . ?
C6 C7 C8 C9 0.0(3) . . . . ?
C4 C7 C8 C9 172.4(2) . . . . ?
C7 C8 C9 S2 0.2(2) . . . . ?
C6 S2 C9 C8 -0.20(17) . . . . ?
O1 B1 C10 C15 -79.2(2) . . . . ?
C5 B1 C10 C15 98.7(3) . . . . ?
O1 B1 C10 C11 98.6(2) . . . . ?
C5 B1 C10 C11 -83.4(3) . . . . ?
C15 C10 C11 C12 1.5(3) . . . . ?
B1 C10 C11 C12 -176.35(19) . . . . ?
C15 C10 C11 C16 -177.8(2) . . . . ?
B1 C10 C11 C16 4.3(3) . . . . ?
C10 C11 C12 C13 -0.7(3) . . . . ?
C16 C11 C12 C13 178.6(2) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C11 C12 C13 C17 -177.9(2) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C17 C13 C14 C15 177.9(2) . . . . ?
C13 C14 C15 C10 0.9(3) . . . . ?
C13 C14 C15 C18 -178.4(2) . . . . ?
C11 C10 C15 C14 -1.6(3) . . . . ?
B1 C10 C15 C14 176.3(2) . . . . ?
C11 C10 C15 C18 177.6(2) . . . . ?
B1 C10 C15 C18 -4.5(3) . . . . ?

_refine_diff_density_max         0.269
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.057


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

data_7_wa3335
_database_code_depnum_ccdc_archive 'CCDC 2384687'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_7_wa3335            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         48 Note  
RESPONSE: These reflections are hidden by the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H12 O S4'
_chemical_formula_sum            'C21 H12 O S4'
_chemical_formula_weight         408.55

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                   15.1300(11)
_cell_length_b                   15.3597(9)
_cell_length_c                   17.5595(16)
_cell_angle_alpha                102.360(7)
_cell_angle_beta                 108.006(8)
_cell_angle_gamma                102.859(6)
_cell_volume                     3603.2(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2669
_cell_measurement_theta_min      4.0630
_cell_measurement_theta_max      27.4180

_exptl_crystal_description       plate
_exptl_crystal_colour            'light yellowish-brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.535
_shelx_estimated_absorpt_T_min   0.807
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_T_min  0.79117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.6762 2766 32843 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.3238 2750 32843 nmt -1.0002 -0.0014 -0.0020 0.0011 -0.9987 0.0015 0.8682
0.6850 1.0011
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -179.9599° 
around [-0.00 0.00 1.00] (reciprocal) or [0.38 0.30 0.88] (direct)
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            16557
_diffrn_reflns_av_unetI/netI     0.2700
_diffrn_reflns_av_R_equivalents  0.1405
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.744
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             16557
_reflns_number_gt                6590
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0239P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         16557
_refine_ls_number_parameters     942
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.0925
_refine_ls_wR_factor_gt          0.0772
_refine_ls_goodness_of_fit_ref   0.738
_refine_ls_restrained_S_all      0.738
_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
S1A S 1.04056(15) 0.01765(12) 0.64137(13) 0.0609(6) Uani 1 1 d . . . . .
S2A S 0.62845(15) -0.01552(11) 0.64916(13) 0.0621(6) Uani 1 1 d . . . . .
S3A S 0.96100(13) 0.36968(11) 0.94411(10) 0.0447(5) Uani 1 1 d . . . . .
S4A S 0.83269(12) 0.36425(11) 0.57311(10) 0.0397(5) Uani 1 1 d . . . . .
O1A O 0.5782(4) 0.1346(3) 0.6137(3) 0.0727(17) Uani 1 1 d . . . . .
C1A C 0.4871(5) 0.0943(5) 0.6199(5) 0.075(3) Uani 1 1 d . . . . .
H1AA H 0.456113 0.030609 0.580686 0.113 Uiso 1 1 calc R U . . .
H1AB H 0.444252 0.132625 0.605949 0.113 Uiso 1 1 calc R U . . .
H1AC H 0.498505 0.092150 0.677458 0.113 Uiso 1 1 calc R U . . .
C11A C 1.0290(5) 0.1164(4) 0.6124(4) 0.049(2) Uani 1 1 d . . . . .
H11A H 1.077506 0.154240 0.599190 0.059 Uiso 1 1 calc R U . . .
C12A C 0.9475(5) 0.1350(4) 0.6100(4) 0.0424(18) Uani 1 1 d . . . . .
H12A H 0.930251 0.185912 0.593764 0.051 Uiso 1 1 calc R U . . .
C13A C 0.8879(5) 0.0691(4) 0.6349(4) 0.0317(16) Uani 1 1 d . . . . .
C14A C 0.9275(5) -0.0011(4) 0.6520(4) 0.0400(17) Uani 1 1 d . . . . .
C15A C 0.8818(6) -0.0743(4) 0.6773(4) 0.059(2) Uani 1 1 d . . . . .
H15A H 0.914124 -0.117571 0.693675 0.070 Uiso 1 1 calc R U . . .
C16A C 0.7903(6) -0.0816(4) 0.6777(4) 0.052(2) Uani 1 1 d . . . . .
H16A H 0.756906 -0.131497 0.692415 0.063 Uiso 1 1 calc R U . . .
C17A C 0.7460(5) -0.0144(4) 0.6560(4) 0.0418(18) Uani 1 1 d . . . . .
C18A C 0.7929(5) 0.0620(4) 0.6361(4) 0.0350(17) Uani 1 1 d . . . . .
C19A C 0.7346(5) 0.1230(4) 0.6222(4) 0.0340(17) Uani 1 1 d . . . . .
C20A C 0.6471(5) 0.0916(4) 0.6244(4) 0.050(2) Uani 1 1 d . . . . .
C21A C 0.8871(4) 0.2538(4) 0.9027(4) 0.0392(18) Uani 1 1 d . . . . .
H21A H 0.878666 0.214565 0.936687 0.047 Uiso 1 1 calc R U . . .
C22A C 0.8431(4) 0.2244(4) 0.8194(4) 0.0328(16) Uani 1 1 d . . . . .
H22A H 0.799384 0.163190 0.787936 0.039 Uiso 1 1 calc R U . . .
C23A C 0.8698(4) 0.2972(4) 0.7824(4) 0.0292(15) Uani 1 1 d . . . . .
C24A C 0.9324(4) 0.3799(4) 0.8437(3) 0.0368(17) Uani 1 1 d . . . . .
C25A C 0.9679(4) 0.4629(4) 0.8247(4) 0.0376(17) Uani 1 1 d . . . . .
H25A H 1.010638 0.518637 0.868185 0.045 Uiso 1 1 calc R U . . .
C26A C 0.9393(4) 0.4609(4) 0.7427(4) 0.0365(17) Uani 1 1 d . . . . .
H26A H 0.962179 0.515639 0.728490 0.044 Uiso 1 1 calc R U . . .
C27A C 0.8765(4) 0.3789(4) 0.6797(4) 0.0283(15) Uani 1 1 d . . . . .
C28A C 0.8396(4) 0.2949(4) 0.6964(3) 0.0227(14) Uani 1 1 d . . . . .
C29A C 0.7766(4) 0.2209(4) 0.6219(4) 0.0328(16) Uani 1 1 d . . . . .
C30A C 0.7653(4) 0.2467(4) 0.5509(4) 0.0375(17) Uani 1 1 d . . . . .
H30A H 0.725567 0.205999 0.495760 0.045 Uiso 1 1 calc R U . . .
S1B S 0.60542(14) 0.04735(12) 0.87836(12) 0.0510(5) Uani 1 1 d . . . . .
S2B S 0.19342(12) 0.04123(10) 0.87386(10) 0.0387(5) Uani 1 1 d . . . . .
S3B S 0.27596(15) 0.18798(13) 0.53648(11) 0.0657(6) Uani 1 1 d . . . . .
S4B S 0.44964(12) 0.45319(10) 0.90050(10) 0.0380(5) Uani 1 1 d . . . . .
O1B O 0.1674(3) 0.2075(3) 0.8591(3) 0.0472(13) Uani 1 1 d . . . . .
C1B C 0.0772(4) 0.1763(4) 0.8682(4) 0.056(2) Uani 1 1 d . . . . .
H1BA H 0.037960 0.115569 0.825833 0.083 Uiso 1 1 calc R U . . .
H1BB H 0.041840 0.222098 0.860619 0.083 Uiso 1 1 calc R U . . .
H1BC H 0.089053 0.169772 0.924513 0.083 Uiso 1 1 calc R U . . .
C11B C 0.6126(5) 0.1566(4) 0.8638(4) 0.0418(19) Uani 1 1 d . . . . .
H11B H 0.667430 0.194301 0.857809 0.050 Uiso 1 1 calc R U . . .
C12B C 0.5325(4) 0.1827(4) 0.8618(3) 0.0349(17) Uani 1 1 d . . . . .
H12B H 0.525353 0.240720 0.854819 0.042 Uiso 1 1 calc R U . . .
C13B C 0.4593(5) 0.1129(4) 0.8716(4) 0.0299(16) Uani 1 1 d . . . . .
C14B C 0.4903(4) 0.0351(4) 0.8814(4) 0.0348(16) Uani 1 1 d . . . . .
C15B C 0.4293(5) -0.0447(4) 0.8914(4) 0.0476(19) Uani 1 1 d . . . . .
H15B H 0.451845 -0.096182 0.899838 0.057 Uiso 1 1 calc R U . . .
C16B C 0.3390(5) -0.0443(4) 0.8884(4) 0.0432(19) Uani 1 1 d . . . . .
H16B H 0.297007 -0.097018 0.893376 0.052 Uiso 1 1 calc R U . . .
C17B C 0.3069(4) 0.0304(4) 0.8784(4) 0.0301(16) Uani 1 1 d . . . . .
C18B C 0.3659(4) 0.1121(4) 0.8720(3) 0.0262(15) Uani 1 1 d . . . . .
C19B C 0.3193(4) 0.1826(3) 0.8650(3) 0.0235(15) Uani 1 1 d . . . . .
C20B C 0.2274(5) 0.1554(4) 0.8670(4) 0.0342(17) Uani 1 1 d . . . . .
C21B C 0.2456(5) 0.1006(4) 0.5804(4) 0.051(2) Uani 1 1 d . . . . .
H21B H 0.212309 0.036611 0.548646 0.061 Uiso 1 1 calc R U . . .
C22B C 0.2746(4) 0.1334(4) 0.6648(4) 0.0353(16) Uani 1 1 d . . . . .
H22B H 0.263743 0.094780 0.698731 0.042 Uiso 1 1 calc R U . . .
C23B C 0.3243(4) 0.2345(4) 0.6984(4) 0.0298(16) Uani 1 1 d . . . . .
C24B C 0.3303(5) 0.2705(4) 0.6345(4) 0.0419(18) Uani 1 1 d . . . . .
C25B C 0.3770(5) 0.3688(4) 0.6496(4) 0.055(2) Uani 1 1 d . . . . .
H25B H 0.379384 0.392877 0.604478 0.066 Uiso 1 1 calc R U . . .
C26B C 0.4184(4) 0.4269(4) 0.7324(4) 0.0408(18) Uani 1 1 d . . . . .
H26B H 0.452732 0.491270 0.745298 0.049 Uiso 1 1 calc R U . . .
C27B C 0.4089(4) 0.3895(4) 0.7961(3) 0.0279(16) Uani 1 1 d . . . . .
C28B C 0.3626(4) 0.2956(4) 0.7822(3) 0.0213(14) Uani 1 1 d . . . . .
C29B C 0.3618(4) 0.2755(3) 0.8580(3) 0.0223(14) Uani 1 1 d . . . . .
C30B C 0.4050(4) 0.3527(4) 0.9253(4) 0.0323(16) Uani 1 1 d . . . . .
H30B H 0.410618 0.352439 0.980616 0.039 Uiso 1 1 calc R U . . .
S1C S 0.49543(12) 0.76471(11) 0.66756(11) 0.0443(5) Uani 1 1 d . . . . .
S2C S 0.08950(13) 0.79643(10) 0.65153(11) 0.0427(5) Uani 1 1 d . . . . .
S3C S 0.26650(13) 0.60947(11) 0.96210(10) 0.0461(5) Uani 1 1 d . . . . .
S4C S 0.09684(12) 0.36444(10) 0.59049(10) 0.0394(5) Uani 1 1 d . . . . .
O1C O -0.0259(3) 0.6247(2) 0.6360(2) 0.0347(11) Uani 1 1 d . . . . .
C1C C -0.0977(4) 0.6700(4) 0.6398(4) 0.0479(19) Uani 1 1 d . . . . .
H1CA H -0.119349 0.689545 0.589407 0.072 Uiso 1 1 calc R U . . .
H1CB H -0.069396 0.725123 0.689871 0.072 Uiso 1 1 calc R U . . .
H1CC H -0.153709 0.626370 0.642887 0.072 Uiso 1 1 calc R U . . .
C11C C 0.4422(4) 0.6471(4) 0.6520(4) 0.0391(17) Uani 1 1 d . . . . .
H11C H 0.475828 0.601956 0.648538 0.047 Uiso 1 1 calc R U . . .
C12C C 0.3490(4) 0.6262(4) 0.6455(3) 0.0312(16) Uani 1 1 d . . . . .
H12C H 0.310000 0.564503 0.636580 0.037 Uiso 1 1 calc R U . . .
C13C C 0.3135(4) 0.7052(4) 0.6530(3) 0.0249(15) Uani 1 1 d . . . . .
C14C C 0.3878(4) 0.7882(4) 0.6659(3) 0.0329(16) Uani 1 1 d . . . . .
C15C C 0.3719(5) 0.8755(4) 0.6745(4) 0.0454(19) Uani 1 1 d . . . . .
H15C H 0.423412 0.929850 0.683826 0.054 Uiso 1 1 calc R U . . .
C16C C 0.2828(5) 0.8819(4) 0.6693(4) 0.0365(18) Uani 1 1 d . . . . .
H16C H 0.270595 0.940478 0.673834 0.044 Uiso 1 1 calc R U . . .
C17C C 0.2074(4) 0.8003(4) 0.6570(4) 0.0307(16) Uani 1 1 d . . . . .
C18C C 0.2213(4) 0.7121(4) 0.6479(4) 0.0270(15) Uani 1 1 d . . . . .
C19C C 0.1352(4) 0.6420(4) 0.6396(3) 0.0231(14) Uani 1 1 d . . . . .
C20C C 0.0618(4) 0.6760(4) 0.6401(3) 0.0288(15) Uani 1 1 d . . . . .
C21C C 0.2638(4) 0.7031(4) 0.9214(4) 0.0349(17) Uani 1 1 d . . . . .
H21C H 0.286950 0.767020 0.954702 0.042 Uiso 1 1 calc R U . . .
C22C C 0.2246(4) 0.6733(4) 0.8366(3) 0.0266(15) Uani 1 1 d . . . . .
H22C H 0.214989 0.714614 0.803727 0.032 Uiso 1 1 calc R U . . .
C23C C 0.1986(4) 0.5730(3) 0.8002(4) 0.0231(14) Uani 1 1 d . . . . .
C24C C 0.2175(4) 0.5286(4) 0.8619(4) 0.0311(16) Uani 1 1 d . . . . .
C25C C 0.1974(4) 0.4320(4) 0.8436(4) 0.0418(18) Uani 1 1 d . . . . .
H25C H 0.208365 0.404099 0.887660 0.050 Uiso 1 1 calc R U . . .
C26C C 0.1618(4) 0.3776(4) 0.7618(4) 0.0363(17) Uani 1 1 d . . . . .
H26C H 0.149742 0.311725 0.748459 0.044 Uiso 1 1 calc R U . . .
C27C C 0.1429(4) 0.4200(4) 0.6970(4) 0.0283(15) Uani 1 1 d . . . . .
C28C C 0.1594(4) 0.5174(3) 0.7149(3) 0.0171(13) Uani 1 1 d . . . . .
C29C C 0.1311(4) 0.5431(4) 0.6398(3) 0.0223(14) Uani 1 1 d . . . . .
C30C C 0.0965(4) 0.4691(4) 0.5688(4) 0.0328(16) Uani 1 1 d . . . . .
H30C H 0.074540 0.474251 0.513583 0.039 Uiso 1 1 calc R U . . .
S1D S 1.05375(12) 0.83004(11) 0.88277(11) 0.0472(5) Uani 1 1 d . . . . .
S2D S 0.65457(12) 0.83398(10) 0.90609(10) 0.0373(5) Uani 1 1 d . . . . .
S3D S 0.63089(12) 0.54919(11) 0.52688(10) 0.0440(5) Uani 1 1 d . . . . .
S4D S 0.67802(13) 0.40883(10) 0.83583(10) 0.0408(5) Uani 1 1 d . . . . .
O1D O 0.5434(3) 0.6542(2) 0.8722(2) 0.0334(11) Uani 1 1 d . . . . .
C1D C 0.4693(4) 0.6963(4) 0.8784(4) 0.0368(16) Uani 1 1 d . . . . .
H1DA H 0.453278 0.726099 0.834067 0.055 Uiso 1 1 calc R U . . .
H1DB H 0.493431 0.743585 0.933509 0.055 Uiso 1 1 calc R U . . .
H1DC H 0.410675 0.647898 0.871895 0.055 Uiso 1 1 calc R U . . .
C11D C 1.0094(4) 0.7106(4) 0.8651(4) 0.0368(17) Uani 1 1 d . . . . .
H11D H 1.045817 0.668830 0.857015 0.044 Uiso 1 1 calc R U . . .
C12D C 0.9183(4) 0.6831(4) 0.8641(3) 0.0356(17) Uani 1 1 d . . . . .
H12D H 0.883569 0.619724 0.854932 0.043 Uiso 1 1 calc R U . . .
C13D C 0.8784(4) 0.7592(4) 0.8782(3) 0.0302(16) Uani 1 1 d . . . . .
C14D C 0.9475(4) 0.8474(4) 0.8903(4) 0.0353(17) Uani 1 1 d . . . . .
C15D C 0.9248(5) 0.9291(4) 0.9054(3) 0.0369(18) Uani 1 1 d . . . . .
H15D H 0.970675 0.985953 0.911252 0.044 Uiso 1 1 calc R U . . .
C16D C 0.8369(4) 0.9308(4) 0.9122(4) 0.0365(17) Uani 1 1 d . . . . .
H16D H 0.822590 0.988200 0.924478 0.044 Uiso 1 1 calc R U . . .
C17D C 0.7704(4) 0.8472(4) 0.9007(3) 0.0303(16) Uani 1 1 d . . . . .
C18D C 0.7862(4) 0.7602(4) 0.8833(3) 0.0257(15) Uani 1 1 d . . . . .
C19D C 0.7058(4) 0.6824(4) 0.8708(3) 0.0244(15) Uani 1 1 d . . . . .
C20D C 0.6302(5) 0.7124(4) 0.8812(3) 0.0314(16) Uani 1 1 d . . . . .
C21D C 0.6592(4) 0.6570(4) 0.5970(4) 0.0349(17) Uani 1 1 d . . . . .
H21D H 0.663261 0.712711 0.581215 0.042 Uiso 1 1 calc R U . . .
C22D C 0.6750(4) 0.6559(4) 0.6758(4) 0.0287(15) Uani 1 1 d . . . . .
H22D H 0.690658 0.710105 0.721548 0.034 Uiso 1 1 calc R U . . .
C23D C 0.6655(4) 0.5632(4) 0.6837(4) 0.0272(15) Uani 1 1 d . . . . .
C24D C 0.6392(4) 0.4970(4) 0.6070(4) 0.0294(16) Uani 1 1 d . . . . .
C25D C 0.6230(4) 0.3996(4) 0.5948(4) 0.0393(18) Uani 1 1 d . . . . .
H25D H 0.604356 0.356885 0.540462 0.047 Uiso 1 1 calc R U . . .
C26D C 0.6353(4) 0.3690(4) 0.6648(4) 0.0333(16) Uani 1 1 d . . . . .
H26D H 0.626325 0.304695 0.660530 0.040 Uiso 1 1 calc R U . . .
C27D C 0.6616(4) 0.4368(4) 0.7425(3) 0.0285(15) Uani 1 1 d . . . . .
C28D C 0.6755(4) 0.5321(3) 0.7555(3) 0.0205(13) Uani 1 1 d . . . . .
C29D C 0.6940(4) 0.5814(3) 0.8400(3) 0.0216(14) Uani 1 1 d . . . . .
C30D C 0.6979(4) 0.5235(4) 0.8895(4) 0.0358(17) Uani 1 1 d . . . . .
H30D H 0.710493 0.544581 0.947890 0.043 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1A C11A 1.728(6) . ?
S1A C14A 1.745(6) . ?
S2A C17A 1.741(7) . ?
S2A C20A 1.775(6) . ?
S3A C24A 1.732(6) . ?
S3A C21A 1.733(5) . ?
S4A C27A 1.726(6) . ?
S4A C30A 1.756(5) . ?
O1A C20A 1.339(7) . ?
O1A C1A 1.427(6) . ?
C1A H1AA 0.9800 . ?
C1A H1AB 0.9800 . ?
C1A H1AC 0.9800 . ?
C11A C12A 1.317(8) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.433(7) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.386(8) . ?
C13A C18A 1.425(8) . ?
C14A C15A 1.413(8) . ?
C15A C16A 1.367(8) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.406(8) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.400(7) . ?
C18A C19A 1.431(8) . ?
C19A C20A 1.321(8) . ?
C19A C29A 1.499(7) . ?
C21A C22A 1.329(7) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.452(7) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.385(7) . ?
C23A C28A 1.427(7) . ?
C24A C25A 1.419(7) . ?
C25A C26A 1.360(7) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.391(7) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.415(7) . ?
C28A C29A 1.421(7) . ?
C29A C30A 1.361(7) . ?
C30A H30A 0.9500 . ?
S1B C14B 1.728(6) . ?
S1B C11B 1.735(6) . ?
S2B C17B 1.740(6) . ?
S2B C20B 1.755(5) . ?
S3B C24B 1.724(6) . ?
S3B C21B 1.730(6) . ?
S4B C27B 1.721(5) . ?
S4B C30B 1.741(5) . ?
O1B C20B 1.332(7) . ?
O1B C1B 1.413(6) . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C11B C12B 1.351(8) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.440(7) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.403(8) . ?
C13B C18B 1.413(8) . ?
C14B C15B 1.440(7) . ?
C15B C16B 1.353(8) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.365(7) . ?
C16B H16B 0.9500 . ?
C17B C18B 1.418(7) . ?
C18B C19B 1.424(7) . ?
C19B C20B 1.374(7) . ?
C19B C29B 1.477(6) . ?
C21B C22B 1.349(7) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.463(7) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.371(7) . ?
C23B C28B 1.421(7) . ?
C24B C25B 1.445(7) . ?
C25B C26B 1.391(7) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.393(7) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.388(6) . ?
C28B C29B 1.431(7) . ?
C29B C30B 1.344(6) . ?
C30B H30B 0.9500 . ?
S1C C11C 1.729(5) . ?
S1C C14C 1.738(6) . ?
S2C C17C 1.744(6) . ?
S2C C20C 1.755(5) . ?
S3C C21C 1.740(6) . ?
S3C C24C 1.742(6) . ?
S4C C27C 1.720(6) . ?
S4C C30C 1.731(5) . ?
O1C C20C 1.355(6) . ?
O1C C1C 1.424(6) . ?
C1C H1CA 0.9800 . ?
C1C H1CB 0.9800 . ?
C1C H1CC 0.9800 . ?
C11C C12C 1.336(7) . ?
C11C H11C 0.9500 . ?
C12C C13C 1.430(7) . ?
C12C H12C 0.9500 . ?
C13C C18C 1.399(7) . ?
C13C C14C 1.422(7) . ?
C14C C15C 1.399(8) . ?
C15C C16C 1.351(8) . ?
C15C H15C 0.9500 . ?
C16C C17C 1.418(7) . ?
C16C H16C 0.9500 . ?
C17C C18C 1.400(7) . ?
C18C C19C 1.438(7) . ?
C19C C20C 1.331(7) . ?
C19C C29C 1.506(7) . ?
C21C C22C 1.350(7) . ?
C21C H21C 0.9500 . ?
C22C C23C 1.447(7) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.390(7) . ?
C23C C28C 1.414(7) . ?
C24C C25C 1.391(7) . ?
C25C C26C 1.363(7) . ?
C25C H25C 0.9500 . ?
C26C C27C 1.415(7) . ?
C26C H26C 0.9500 . ?
C27C C28C 1.408(7) . ?
C28C C29C 1.424(7) . ?
C29C C30C 1.358(7) . ?
C30C H30C 0.9500 . ?
S1D C14D 1.726(6) . ?
S1D C11D 1.729(5) . ?
S2D C20D 1.749(5) . ?
S2D C17D 1.753(6) . ?
S3D C21D 1.711(6) . ?
S3D C24D 1.748(6) . ?
S4D C30D 1.720(5) . ?
S4D C27D 1.741(5) . ?
O1D C20D 1.355(6) . ?
O1D C1D 1.433(6) . ?
C1D H1DA 0.9800 . ?
C1D H1DB 0.9800 . ?
C1D H1DC 0.9800 . ?
C11D C12D 1.342(7) . ?
C11D H11D 0.9500 . ?
C12D C13D 1.441(7) . ?
C12D H12D 0.9500 . ?
C13D C18D 1.428(8) . ?
C13D C14D 1.443(7) . ?
C14D C15D 1.368(7) . ?
C15D C16D 1.377(7) . ?
C15D H15D 0.9500 . ?
C16D C17D 1.375(7) . ?
C16D H16D 0.9500 . ?
C17D C18D 1.397(7) . ?
C18D C19D 1.425(7) . ?
C19D C20D 1.371(7) . ?
C19D C29D 1.479(7) . ?
C21D C22D 1.334(7) . ?
C21D H21D 0.9500 . ?
C22D C23D 1.439(7) . ?
C22D H22D 0.9500 . ?
C23D C24D 1.382(7) . ?
C23D C28D 1.418(7) . ?
C24D C25D 1.418(7) . ?
C25D C26D 1.382(7) . ?
C25D H25D 0.9500 . ?
C26D C27D 1.406(7) . ?
C26D H26D 0.9500 . ?
C27D C28D 1.390(7) . ?
C28D C29D 1.421(7) . ?
C29D C30D 1.369(7) . ?
C30D H30D 0.9500 . ?

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
C11A S1A C14A 90.3(3) . . ?
C17A S2A C20A 89.8(3) . . ?
C24A S3A C21A 90.0(3) . . ?
C27A S4A C30A 91.6(3) . . ?
C20A O1A C1A 120.9(5) . . ?
O1A C1A H1AA 109.5 . . ?
O1A C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
O1A C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C12A C11A S1A 114.5(5) . . ?
C12A C11A H11A 122.7 . . ?
S1A C11A H11A 122.7 . . ?
C11A C12A C13A 111.9(6) . . ?
C11A C12A H12A 124.1 . . ?
C13A C12A H12A 124.1 . . ?
C14A C13A C18A 118.0(6) . . ?
C14A C13A C12A 112.8(6) . . ?
C18A C13A C12A 129.0(6) . . ?
C13A C14A C15A 123.2(7) . . ?
C13A C14A S1A 110.4(5) . . ?
C15A C14A S1A 126.3(6) . . ?
C16A C15A C14A 118.6(7) . . ?
C16A C15A H15A 120.7 . . ?
C14A C15A H15A 120.7 . . ?
C15A C16A C17A 119.2(6) . . ?
C15A C16A H16A 120.4 . . ?
C17A C16A H16A 120.4 . . ?
C18A C17A C16A 122.8(6) . . ?
C18A C17A S2A 111.9(5) . . ?
C16A C17A S2A 125.3(6) . . ?
C17A C18A C13A 117.9(6) . . ?
C17A C18A C19A 111.4(6) . . ?
C13A C18A C19A 130.6(5) . . ?
C20A C19A C18A 113.9(6) . . ?
C20A C19A C29A 123.0(6) . . ?
C18A C19A C29A 122.1(6) . . ?
C19A C20A O1A 126.3(6) . . ?
C19A C20A S2A 112.8(5) . . ?
O1A C20A S2A 120.8(5) . . ?
C22A C21A S3A 114.4(5) . . ?
C22A C21A H21A 122.8 . . ?
S3A C21A H21A 122.8 . . ?
C21A C22A C23A 111.9(5) . . ?
C21A C22A H22A 124.1 . . ?
C23A C22A H22A 124.1 . . ?
C24A C23A C28A 118.9(5) . . ?
C24A C23A C22A 111.2(5) . . ?
C28A C23A C22A 129.9(5) . . ?
C23A C24A C25A 122.8(5) . . ?
C23A C24A S3A 112.4(5) . . ?
C25A C24A S3A 124.8(4) . . ?
C26A C25A C24A 118.5(5) . . ?
C26A C25A H25A 120.8 . . ?
C24A C25A H25A 120.8 . . ?
C25A C26A C27A 120.1(5) . . ?
C25A C26A H26A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C26A C27A C28A 123.0(5) . . ?
C26A C27A S4A 126.2(4) . . ?
C28A C27A S4A 110.9(4) . . ?
C27A C28A C29A 112.5(5) . . ?
C27A C28A C23A 116.8(5) . . ?
C29A C28A C23A 130.6(5) . . ?
C30A C29A C28A 113.0(5) . . ?
C30A C29A C19A 124.0(5) . . ?
C28A C29A C19A 122.8(5) . . ?
C29A C30A S4A 112.0(4) . . ?
C29A C30A H30A 124.0 . . ?
S4A C30A H30A 124.0 . . ?
C14B S1B C11B 90.6(3) . . ?
C17B S2B C20B 91.0(3) . . ?
C24B S3B C21B 90.8(3) . . ?
C27B S4B C30B 90.8(3) . . ?
C20B O1B C1B 119.5(5) . . ?
O1B C1B H1BA 109.5 . . ?
O1B C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
O1B C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C12B C11B S1B 113.5(5) . . ?
C12B C11B H11B 123.3 . . ?
S1B C11B H11B 123.3 . . ?
C11B C12B C13B 112.5(6) . . ?
C11B C12B H12B 123.7 . . ?
C13B C12B H12B 123.7 . . ?
C14B C13B C18B 118.6(5) . . ?
C14B C13B C12B 111.0(6) . . ?
C18B C13B C12B 130.4(6) . . ?
C13B C14B C15B 121.6(6) . . ?
C13B C14B S1B 112.4(5) . . ?
C15B C14B S1B 126.1(5) . . ?
C16B C15B C14B 118.1(6) . . ?
C16B C15B H15B 120.9 . . ?
C14B C15B H15B 120.9 . . ?
C15B C16B C17B 121.4(6) . . ?
C15B C16B H16B 119.3 . . ?
C17B C16B H16B 119.3 . . ?
C16B C17B C18B 122.5(6) . . ?
C16B C17B S2B 126.6(5) . . ?
C18B C17B S2B 110.9(5) . . ?
C13B C18B C17B 117.8(5) . . ?
C13B C18B C19B 129.0(5) . . ?
C17B C18B C19B 113.2(5) . . ?
C20B C19B C18B 111.8(5) . . ?
C20B C19B C29B 122.0(5) . . ?
C18B C19B C29B 126.1(5) . . ?
O1B C20B C19B 123.8(5) . . ?
O1B C20B S2B 123.1(5) . . ?
C19B C20B S2B 113.0(4) . . ?
C22B C21B S3B 112.6(4) . . ?
C22B C21B H21B 123.7 . . ?
S3B C21B H21B 123.7 . . ?
C21B C22B C23B 113.0(5) . . ?
C21B C22B H22B 123.5 . . ?
C23B C22B H22B 123.5 . . ?
C24B C23B C28B 119.5(5) . . ?
C24B C23B C22B 110.0(5) . . ?
C28B C23B C22B 130.5(5) . . ?
C23B C24B C25B 122.1(5) . . ?
C23B C24B S3B 113.6(4) . . ?
C25B C24B S3B 124.3(5) . . ?
C26B C25B C24B 117.7(5) . . ?
C26B C25B H25B 121.2 . . ?
C24B C25B H25B 121.2 . . ?
C25B C26B C27B 119.3(5) . . ?
C25B C26B H26B 120.4 . . ?
C27B C26B H26B 120.4 . . ?
C28B C27B C26B 123.5(5) . . ?
C28B C27B S4B 111.6(4) . . ?
C26B C27B S4B 124.9(4) . . ?
C27B C28B C23B 117.9(5) . . ?
C27B C28B C29B 112.4(5) . . ?
C23B C28B C29B 129.7(5) . . ?
C30B C29B C28B 112.1(5) . . ?
C30B C29B C19B 121.9(5) . . ?
C28B C29B C19B 126.0(5) . . ?
C29B C30B S4B 113.0(4) . . ?
C29B C30B H30B 123.5 . . ?
S4B C30B H30B 123.5 . . ?
C11C S1C C14C 91.1(3) . . ?
C17C S2C C20C 89.5(3) . . ?
C21C S3C C24C 92.0(3) . . ?
C27C S4C C30C 91.5(3) . . ?
C20C O1C C1C 118.7(4) . . ?
O1C C1C H1CA 109.5 . . ?
O1C C1C H1CB 109.5 . . ?
H1CA C1C H1CB 109.5 . . ?
O1C C1C H1CC 109.5 . . ?
H1CA C1C H1CC 109.5 . . ?
H1CB C1C H1CC 109.5 . . ?
C12C C11C S1C 113.2(5) . . ?
C12C C11C H11C 123.4 . . ?
S1C C11C H11C 123.4 . . ?
C11C C12C C13C 113.9(5) . . ?
C11C C12C H12C 123.1 . . ?
C13C C12C H12C 123.1 . . ?
C18C C13C C14C 118.1(5) . . ?
C18C C13C C12C 131.2(5) . . ?
C14C C13C C12C 110.7(5) . . ?
C15C C14C C13C 122.4(6) . . ?
C15C C14C S1C 126.5(5) . . ?
C13C C14C S1C 111.1(5) . . ?
C16C C15C C14C 119.4(5) . . ?
C16C C15C H15C 120.3 . . ?
C14C C15C H15C 120.3 . . ?
C15C C16C C17C 119.5(6) . . ?
C15C C16C H16C 120.3 . . ?
C17C C16C H16C 120.3 . . ?
C18C C17C C16C 122.3(6) . . ?
C18C C17C S2C 112.3(4) . . ?
C16C C17C S2C 125.5(5) . . ?
C13C C18C C17C 118.4(5) . . ?
C13C C18C C19C 130.1(5) . . ?
C17C C18C C19C 111.4(5) . . ?
C20C C19C C18C 112.7(5) . . ?
C20C C19C C29C 122.9(5) . . ?
C18C C19C C29C 124.1(5) . . ?
C19C C20C O1C 124.0(5) . . ?
C19C C20C S2C 114.1(4) . . ?
O1C C20C S2C 121.9(4) . . ?
C22C C21C S3C 111.3(4) . . ?
C22C C21C H21C 124.3 . . ?
S3C C21C H21C 124.3 . . ?
C21C C22C C23C 114.1(5) . . ?
C21C C22C H22C 123.0 . . ?
C23C C22C H22C 123.0 . . ?
C24C C23C C28C 118.4(5) . . ?
C24C C23C C22C 111.4(5) . . ?
C28C C23C C22C 130.1(5) . . ?
C23C C24C C25C 123.0(6) . . ?
C23C C24C S3C 111.1(4) . . ?
C25C C24C S3C 125.9(5) . . ?
C26C C25C C24C 119.3(6) . . ?
C26C C25C H25C 120.4 . . ?
C24C C25C H25C 120.4 . . ?
C25C C26C C27C 119.6(5) . . ?
C25C C26C H26C 120.2 . . ?
C27C C26C H26C 120.2 . . ?
C28C C27C C26C 121.4(5) . . ?
C28C C27C S4C 111.6(4) . . ?
C26C C27C S4C 126.9(5) . . ?
C27C C28C C23C 118.2(5) . . ?
C27C C28C C29C 111.3(5) . . ?
C23C C28C C29C 130.5(5) . . ?
C30C C29C C28C 113.2(5) . . ?
C30C C29C C19C 123.6(5) . . ?
C28C C29C C19C 123.1(5) . . ?
C29C C30C S4C 112.3(4) . . ?
C29C C30C H30C 123.9 . . ?
S4C C30C H30C 123.9 . . ?
C14D S1D C11D 92.4(3) . . ?
C20D S2D C17D 90.6(3) . . ?
C21D S3D C24D 90.6(3) . . ?
C30D S4D C27D 90.7(3) . . ?
C20D O1D C1D 116.8(4) . . ?
O1D C1D H1DA 109.5 . . ?
O1D C1D H1DB 109.5 . . ?
H1DA C1D H1DB 109.5 . . ?
O1D C1D H1DC 109.5 . . ?
H1DA C1D H1DC 109.5 . . ?
H1DB C1D H1DC 109.5 . . ?
C12D C11D S1D 113.1(5) . . ?
C12D C11D H11D 123.5 . . ?
S1D C11D H11D 123.5 . . ?
C11D C12D C13D 113.3(5) . . ?
C11D C12D H12D 123.4 . . ?
C13D C12D H12D 123.4 . . ?
C18D C13D C12D 130.9(5) . . ?
C18D C13D C14D 118.0(6) . . ?
C12D C13D C14D 111.1(6) . . ?
C15D C14D C13D 120.8(6) . . ?
C15D C14D S1D 129.0(5) . . ?
C13D C14D S1D 110.2(5) . . ?
C14D C15D C16D 121.5(5) . . ?
C14D C15D H15D 119.3 . . ?
C16D C15D H15D 119.3 . . ?
C17D C16D C15D 118.2(6) . . ?
C17D C16D H16D 120.9 . . ?
C15D C16D H16D 120.9 . . ?
C16D C17D C18D 124.4(6) . . ?
C16D C17D S2D 125.4(5) . . ?
C18D C17D S2D 110.2(4) . . ?
C17D C18D C19D 114.8(6) . . ?
C17D C18D C13D 117.0(5) . . ?
C19D C18D C13D 128.1(6) . . ?
C20D C19D C18D 110.4(5) . . ?
C20D C19D C29D 121.3(5) . . ?
C18D C19D C29D 127.9(5) . . ?
O1D C20D C19D 123.9(5) . . ?
O1D C20D S2D 122.1(5) . . ?
C19D C20D S2D 113.9(4) . . ?
C22D C21D S3D 114.1(5) . . ?
C22D C21D H21D 122.9 . . ?
S3D C21D H21D 122.9 . . ?
C21D C22D C23D 112.3(5) . . ?
C21D C22D H22D 123.8 . . ?
C23D C22D H22D 123.8 . . ?
C24D C23D C28D 118.2(5) . . ?
C24D C23D C22D 111.8(5) . . ?
C28D C23D C22D 130.0(5) . . ?
C23D C24D C25D 124.6(5) . . ?
C23D C24D S3D 111.1(4) . . ?
C25D C24D S3D 124.2(5) . . ?
C26D C25D C24D 117.6(5) . . ?
C26D C25D H25D 121.2 . . ?
C24D C25D H25D 121.2 . . ?
C25D C26D C27D 117.4(5) . . ?
C25D C26D H26D 121.3 . . ?
C27D C26D H26D 121.3 . . ?
C28D C27D C26D 126.0(5) . . ?
C28D C27D S4D 111.3(4) . . ?
C26D C27D S4D 122.7(4) . . ?
C27D C28D C23D 116.2(5) . . ?
C27D C28D C29D 112.7(5) . . ?
C23D C28D C29D 131.1(5) . . ?
C30D C29D C28D 111.6(5) . . ?
C30D C29D C19D 123.8(5) . . ?
C28D C29D C19D 124.5(5) . . ?
C29D C30D S4D 113.5(4) . . ?
C29D C30D H30D 123.2 . . ?
S4D C30D H30D 123.2 . . ?

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
C14A S1A C11A C12A -0.3(6) . . . . ?
S1A C11A C12A C13A 1.7(8) . . . . ?
C11A C12A C13A C14A -2.7(8) . . . . ?
C11A C12A C13A C18A -176.1(6) . . . . ?
C18A C13A C14A C15A -5.5(9) . . . . ?
C12A C13A C14A C15A -179.7(5) . . . . ?
C18A C13A C14A S1A 176.6(4) . . . . ?
C12A C13A C14A S1A 2.5(7) . . . . ?
C11A S1A C14A C13A -1.3(5) . . . . ?
C11A S1A C14A C15A -179.1(6) . . . . ?
C13A C14A C15A C16A 6.2(10) . . . . ?
S1A C14A C15A C16A -176.3(5) . . . . ?
C14A C15A C16A C17A -2.3(10) . . . . ?
C15A C16A C17A C18A -1.9(10) . . . . ?
C15A C16A C17A S2A 177.3(5) . . . . ?
C20A S2A C17A C18A -2.7(5) . . . . ?
C20A S2A C17A C16A 178.0(6) . . . . ?
C16A C17A C18A C13A 2.5(9) . . . . ?
S2A C17A C18A C13A -176.8(4) . . . . ?
C16A C17A C18A C19A -176.0(6) . . . . ?
S2A C17A C18A C19A 4.7(7) . . . . ?
C14A C13A C18A C17A 1.1(9) . . . . ?
C12A C13A C18A C17A 174.2(6) . . . . ?
C14A C13A C18A C19A 179.3(6) . . . . ?
C12A C13A C18A C19A -7.6(11) . . . . ?
C17A C18A C19A C20A -4.9(8) . . . . ?
C13A C18A C19A C20A 176.9(6) . . . . ?
C17A C18A C19A C29A 163.9(5) . . . . ?
C13A C18A C19A C29A -14.3(10) . . . . ?
C18A C19A C20A O1A 179.7(7) . . . . ?
C29A C19A C20A O1A 11.0(12) . . . . ?
C18A C19A C20A S2A 2.8(8) . . . . ?
C29A C19A C20A S2A -165.9(4) . . . . ?
C1A O1A C20A C19A -178.3(7) . . . . ?
C1A O1A C20A S2A -1.6(10) . . . . ?
C17A S2A C20A C19A 0.0(6) . . . . ?
C17A S2A C20A O1A -177.2(6) . . . . ?
C24A S3A C21A C22A -0.4(6) . . . . ?
S3A C21A C22A C23A 1.3(8) . . . . ?
C21A C22A C23A C24A -1.8(8) . . . . ?
C21A C22A C23A C28A 180.0(6) . . . . ?
C28A C23A C24A C25A 0.0(9) . . . . ?
C22A C23A C24A C25A -178.4(6) . . . . ?
C28A C23A C24A S3A 179.9(4) . . . . ?
C22A C23A C24A S3A 1.5(7) . . . . ?
C21A S3A C24A C23A -0.6(5) . . . . ?
C21A S3A C24A C25A 179.3(6) . . . . ?
C23A C24A C25A C26A -0.1(10) . . . . ?
S3A C24A C25A C26A -180.0(5) . . . . ?
C24A C25A C26A C27A 0.1(9) . . . . ?
C25A C26A C27A C28A 0.0(9) . . . . ?
C25A C26A C27A S4A 179.7(5) . . . . ?
C30A S4A C27A C26A -179.6(5) . . . . ?
C30A S4A C27A C28A 0.1(5) . . . . ?
C26A C27A C28A C29A 179.7(6) . . . . ?
S4A C27A C28A C29A -0.1(6) . . . . ?
C26A C27A C28A C23A -0.1(9) . . . . ?
S4A C27A C28A C23A -179.8(4) . . . . ?
C24A C23A C28A C27A 0.1(8) . . . . ?
C22A C23A C28A C27A 178.2(6) . . . . ?
C24A C23A C28A C29A -179.6(6) . . . . ?
C22A C23A C28A C29A -1.5(11) . . . . ?
C27A C28A C29A C30A -0.1(8) . . . . ?
C23A C28A C29A C30A 179.7(6) . . . . ?
C27A C28A C29A C19A 175.0(6) . . . . ?
C23A C28A C29A C19A -5.3(10) . . . . ?
C20A C19A C29A C30A -90.4(9) . . . . ?
C18A C19A C29A C30A 101.9(8) . . . . ?
C20A C19A C29A C28A 95.2(8) . . . . ?
C18A C19A C29A C28A -72.6(8) . . . . ?
C28A C29A C30A S4A 0.2(7) . . . . ?
C19A C29A C30A S4A -174.8(5) . . . . ?
C27A S4A C30A C29A -0.2(5) . . . . ?
C14B S1B C11B C12B 0.4(5) . . . . ?
S1B C11B C12B C13B -0.5(7) . . . . ?
C11B C12B C13B C14B 0.5(8) . . . . ?
C11B C12B C13B C18B -179.1(6) . . . . ?
C18B C13B C14B C15B 0.3(9) . . . . ?
C12B C13B C14B C15B -179.4(5) . . . . ?
C18B C13B C14B S1B 179.4(4) . . . . ?
C12B C13B C14B S1B -0.2(7) . . . . ?
C11B S1B C14B C13B -0.1(5) . . . . ?
C11B S1B C14B C15B 179.0(6) . . . . ?
C13B C14B C15B C16B 2.1(10) . . . . ?
S1B C14B C15B C16B -176.9(5) . . . . ?
C14B C15B C16B C17B -1.7(10) . . . . ?
C15B C16B C17B C18B -1.0(10) . . . . ?
C15B C16B C17B S2B -179.8(5) . . . . ?
C20B S2B C17B C16B 177.0(6) . . . . ?
C20B S2B C17B C18B -1.9(5) . . . . ?
C14B C13B C18B C17B -2.8(9) . . . . ?
C12B C13B C18B C17B 176.7(6) . . . . ?
C14B C13B C18B C19B 178.5(6) . . . . ?
C12B C13B C18B C19B -1.9(11) . . . . ?
C16B C17B C18B C13B 3.3(9) . . . . ?
S2B C17B C18B C13B -177.7(4) . . . . ?
C16B C17B C18B C19B -177.8(6) . . . . ?
S2B C17B C18B C19B 1.1(6) . . . . ?
C13B C18B C19B C20B 179.3(6) . . . . ?
C17B C18B C19B C20B 0.6(7) . . . . ?
C13B C18B C19B C29B -1.8(10) . . . . ?
C17B C18B C19B C29B 179.5(5) . . . . ?
C1B O1B C20B C19B -175.4(6) . . . . ?
C1B O1B C20B S2B 9.1(8) . . . . ?
C18B C19B C20B O1B -178.0(6) . . . . ?
C29B C19B C20B O1B 3.1(9) . . . . ?
C18B C19B C20B S2B -2.0(7) . . . . ?
C29B C19B C20B S2B 179.0(4) . . . . ?
C17B S2B C20B O1B 178.3(5) . . . . ?
C17B S2B C20B C19B 2.3(5) . . . . ?
C24B S3B C21B C22B 0.7(6) . . . . ?
S3B C21B C22B C23B 0.0(8) . . . . ?
C21B C22B C23B C24B -1.0(8) . . . . ?
C21B C22B C23B C28B 177.8(6) . . . . ?
C28B C23B C24B C25B 1.8(10) . . . . ?
C22B C23B C24B C25B -179.3(6) . . . . ?
C28B C23B C24B S3B -177.4(5) . . . . ?
C22B C23B C24B S3B 1.6(7) . . . . ?
C21B S3B C24B C23B -1.3(6) . . . . ?
C21B S3B C24B C25B 179.5(6) . . . . ?
C23B C24B C25B C26B 1.4(10) . . . . ?
S3B C24B C25B C26B -179.6(5) . . . . ?
C24B C25B C26B C27B -3.3(10) . . . . ?
C25B C26B C27B C28B 2.2(10) . . . . ?
C25B C26B C27B S4B -176.2(5) . . . . ?
C30B S4B C27B C28B 0.4(5) . . . . ?
C30B S4B C27B C26B 179.0(6) . . . . ?
C26B C27B C28B C23B 0.9(9) . . . . ?
S4B C27B C28B C23B 179.5(4) . . . . ?
C26B C27B C28B C29B -179.4(6) . . . . ?
S4B C27B C28B C29B -0.8(7) . . . . ?
C24B C23B C28B C27B -2.9(9) . . . . ?
C22B C23B C28B C27B 178.4(6) . . . . ?
C24B C23B C28B C29B 177.5(6) . . . . ?
C22B C23B C28B C29B -1.2(11) . . . . ?
C27B C28B C29B C30B 0.8(8) . . . . ?
C23B C28B C29B C30B -179.5(6) . . . . ?
C27B C28B C29B C19B -179.4(6) . . . . ?
C23B C28B C29B C19B 0.2(10) . . . . ?
C20B C19B C29B C30B 82.2(8) . . . . ?
C18B C19B C29B C30B -96.6(8) . . . . ?
C20B C19B C29B C28B -97.5(8) . . . . ?
C18B C19B C29B C28B 83.7(8) . . . . ?
C28B C29B C30B S4B -0.5(7) . . . . ?
C19B C29B C30B S4B 179.8(4) . . . . ?
C27B S4B C30B C29B 0.0(5) . . . . ?
C14C S1C C11C C12C 0.4(5) . . . . ?
S1C C11C C12C C13C -0.3(7) . . . . ?
C11C C12C C13C C18C 178.3(6) . . . . ?
C11C C12C C13C C14C 0.0(7) . . . . ?
C18C C13C C14C C15C 0.8(9) . . . . ?
C12C C13C C14C C15C 179.3(5) . . . . ?
C18C C13C C14C S1C -178.3(4) . . . . ?
C12C C13C C14C S1C 0.2(6) . . . . ?
C11C S1C C14C C15C -179.3(6) . . . . ?
C11C S1C C14C C13C -0.3(4) . . . . ?
C13C C14C C15C C16C -0.9(9) . . . . ?
S1C C14C C15C C16C 178.0(5) . . . . ?
C14C C15C C16C C17C 1.3(10) . . . . ?
C15C C16C C17C C18C -1.7(10) . . . . ?
C15C C16C C17C S2C 178.3(5) . . . . ?
C20C S2C C17C C18C 1.7(5) . . . . ?
C20C S2C C17C C16C -178.3(5) . . . . ?
C14C C13C C18C C17C -1.1(9) . . . . ?
C12C C13C C18C C17C -179.2(6) . . . . ?
C14C C13C C18C C19C -176.4(5) . . . . ?
C12C C13C C18C C19C 5.4(11) . . . . ?
C16C C17C C18C C13C 1.5(9) . . . . ?
S2C C17C C18C C13C -178.5(4) . . . . ?
C16C C17C C18C C19C 177.7(5) . . . . ?
S2C C17C C18C C19C -2.3(6) . . . . ?
C13C C18C C19C C20C 177.4(6) . . . . ?
C17C C18C C19C C20C 1.8(7) . . . . ?
C13C C18C C19C C29C 3.7(10) . . . . ?
C17C C18C C19C C29C -171.9(5) . . . . ?
C18C C19C C20C O1C -177.8(5) . . . . ?
C29C C19C C20C O1C -4.0(9) . . . . ?
C18C C19C C20C S2C -0.5(7) . . . . ?
C29C C19C C20C S2C 173.3(4) . . . . ?
C1C O1C C20C C19C 178.0(6) . . . . ?
C1C O1C C20C S2C 0.9(7) . . . . ?
C17C S2C C20C C19C -0.7(5) . . . . ?
C17C S2C C20C O1C 176.7(5) . . . . ?
C24C S3C C21C C22C 2.0(5) . . . . ?
S3C C21C C22C C23C -2.5(7) . . . . ?
C21C C22C C23C C24C 1.8(7) . . . . ?
C21C C22C C23C C28C -177.7(6) . . . . ?
C28C C23C C24C C25C -1.6(8) . . . . ?
C22C C23C C24C C25C 178.8(5) . . . . ?
C28C C23C C24C S3C 179.4(4) . . . . ?
C22C C23C C24C S3C -0.2(6) . . . . ?
C21C S3C C24C C23C -1.0(5) . . . . ?
C21C S3C C24C C25C 180.0(5) . . . . ?
C23C C24C C25C C26C 3.2(9) . . . . ?
S3C C24C C25C C26C -177.9(5) . . . . ?
C24C C25C C26C C27C -2.0(9) . . . . ?
C25C C26C C27C C28C -0.5(9) . . . . ?
C25C C26C C27C S4C -179.1(5) . . . . ?
C30C S4C C27C C28C -1.2(4) . . . . ?
C30C S4C C27C C26C 177.5(5) . . . . ?
C26C C27C C28C C23C 2.0(8) . . . . ?
S4C C27C C28C C23C -179.2(4) . . . . ?
C26C C27C C28C C29C -177.4(5) . . . . ?
S4C C27C C28C C29C 1.4(6) . . . . ?
C24C C23C C28C C27C -1.0(8) . . . . ?
C22C C23C C28C C27C 178.5(5) . . . . ?
C24C C23C C28C C29C 178.3(6) . . . . ?
C22C C23C C28C C29C -2.2(10) . . . . ?
C27C C28C C29C C30C -0.9(7) . . . . ?
C23C C28C C29C C30C 179.8(5) . . . . ?
C27C C28C C29C C19C 176.6(5) . . . . ?
C23C C28C C29C C19C -2.7(9) . . . . ?
C20C C19C C29C C30C 89.3(8) . . . . ?
C18C C19C C29C C30C -97.6(7) . . . . ?
C20C C19C C29C C28C -87.9(7) . . . . ?
C18C C19C C29C C28C 85.2(7) . . . . ?
C28C C29C C30C S4C 0.0(6) . . . . ?
C19C C29C C30C S4C -177.5(4) . . . . ?
C27C S4C C30C C29C 0.7(5) . . . . ?
C14D S1D C11D C12D 0.4(5) . . . . ?
S1D C11D C12D C13D -0.2(7) . . . . ?
C11D C12D C13D C18D -178.8(6) . . . . ?
C11D C12D C13D C14D -0.1(7) . . . . ?
C18D C13D C14D C15D -0.6(8) . . . . ?
C12D C13D C14D C15D -179.5(6) . . . . ?
C18D C13D C14D S1D 179.3(4) . . . . ?
C12D C13D C14D S1D 0.4(6) . . . . ?
C11D S1D C14D C15D 179.4(6) . . . . ?
C11D S1D C14D C13D -0.5(4) . . . . ?
C13D C14D C15D C16D 2.1(9) . . . . ?
S1D C14D C15D C16D -177.8(5) . . . . ?
C14D C15D C16D C17D -2.1(9) . . . . ?
C15D C16D C17D C18D 0.7(9) . . . . ?
C15D C16D C17D S2D -179.6(5) . . . . ?
C20D S2D C17D C16D 178.2(5) . . . . ?
C20D S2D C17D C18D -2.0(4) . . . . ?
C16D C17D C18D C19D -177.8(5) . . . . ?
S2D C17D C18D C19D 2.4(6) . . . . ?
C16D C17D C18D C13D 0.7(9) . . . . ?
S2D C17D C18D C13D -179.1(4) . . . . ?
C12D C13D C18D C17D 177.9(6) . . . . ?
C14D C13D C18D C17D -0.7(8) . . . . ?
C12D C13D C18D C19D -3.8(10) . . . . ?
C14D C13D C18D C19D 177.6(5) . . . . ?
C17D C18D C19D C20D -1.5(7) . . . . ?
C13D C18D C19D C20D -179.9(6) . . . . ?
C17D C18D C19D C29D 170.6(5) . . . . ?
C13D C18D C19D C29D -7.8(10) . . . . ?
C1D O1D C20D C19D -175.1(5) . . . . ?
C1D O1D C20D S2D 4.1(7) . . . . ?
C18D C19D C20D O1D 179.2(5) . . . . ?
C29D C19D C20D O1D 6.5(9) . . . . ?
C18D C19D C20D S2D -0.1(6) . . . . ?
C29D C19D C20D S2D -172.8(4) . . . . ?
C17D S2D C20D O1D -178.0(5) . . . . ?
C17D S2D C20D C19D 1.2(5) . . . . ?
C24D S3D C21D C22D 0.5(5) . . . . ?
S3D C21D C22D C23D 0.7(7) . . . . ?
C21D C22D C23D C24D -1.9(7) . . . . ?
C21D C22D C23D C28D -179.4(6) . . . . ?
C28D C23D C24D C25D -1.1(9) . . . . ?
C22D C23D C24D C25D -178.9(5) . . . . ?
C28D C23D C24D S3D -180.0(4) . . . . ?
C22D C23D C24D S3D 2.2(6) . . . . ?
C21D S3D C24D C23D -1.6(5) . . . . ?
C21D S3D C24D C25D 179.6(5) . . . . ?
C23D C24D C25D C26D -0.7(9) . . . . ?
S3D C24D C25D C26D 178.0(5) . . . . ?
C24D C25D C26D C27D 0.9(8) . . . . ?
C25D C26D C27D C28D 0.8(9) . . . . ?
C25D C26D C27D S4D 179.1(5) . . . . ?
C30D S4D C27D C28D 2.3(5) . . . . ?
C30D S4D C27D C26D -176.2(5) . . . . ?
C26D C27D C28D C23D -2.6(9) . . . . ?
S4D C27D C28D C23D 179.0(4) . . . . ?
C26D C27D C28D C29D 175.2(5) . . . . ?
S4D C27D C28D C29D -3.2(6) . . . . ?
C24D C23D C28D C27D 2.6(8) . . . . ?
C22D C23D C28D C27D 179.9(6) . . . . ?
C24D C23D C28D C29D -174.7(6) . . . . ?
C22D C23D C28D C29D 2.7(10) . . . . ?
C27D C28D C29D C30D 2.6(7) . . . . ?
C23D C28D C29D C30D 180.0(6) . . . . ?
C27D C28D C29D C19D -176.3(5) . . . . ?
C23D C28D C29D C19D 1.0(10) . . . . ?
C20D C19D C29D C30D -79.6(8) . . . . ?
C18D C19D C29D C30D 109.1(7) . . . . ?
C20D C19D C29D C28D 99.2(7) . . . . ?
C18D C19D C29D C28D -72.1(8) . . . . ?
C28D C29D C30D S4D -0.8(7) . . . . ?
C19D C29D C30D S4D 178.1(4) . . . . ?
C27D S4D C30D C29D -0.8(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
_geom_hbond_publ_flag
C1A H1AB S3B 0.98 2.86 3.805(8) 162.2 . yes
C26A H26A O1C 0.95 2.59 3.487(7) 158.3 1_655 yes
C25B H25B S3D 0.95 2.62 3.565(6) 174.8 2_666 yes
C30B H30B O1D 0.95 2.49 3.428(7) 168.6 2_667 yes
C30C H30C O1C 0.95 2.52 3.297(7) 139.2 2_566 yes
C26D H26D O1A 0.95 2.43 3.357(7) 165.7 . yes

_refine_diff_density_max         0.305
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.070


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

data_10_wa3194
_database_code_depnum_ccdc_archive 'CCDC 2384690'
loop_
_audit_author_name
_audit_author_address
'Dr. Michael Bolte'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT340_10_wa3194           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01439 Ang.  
RESPONSE: The crystal scattered weakly.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H23 B O S4'
_chemical_formula_sum            'C29 H23 B O S4'
_chemical_formula_weight         526.52

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'
B B 0.0013 0.0007 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   6.3515(5)
_cell_length_b                   18.4915(11)
_cell_length_c                   22.5750(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2651.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    14919
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      26.03

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.379
_shelx_estimated_absorpt_T_min   0.935
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14919
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.332
_diffrn_reflns_theta_max         25.750
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4991
_reflns_number_gt                3786
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.731
_reflns_Friedel_fraction_max     0.978
_reflns_Friedel_fraction_full    1.000

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

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0435P)²+11.1253P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1166 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.19(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4991
_refine_ls_number_parameters     319
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0833
_refine_ls_wR_factor_ref         0.1981
_refine_ls_wR_factor_gt          0.1707
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_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
S1 S -0.2640(4) 0.49662(12) 0.64019(9) 0.0309(5) Uani 1 1 d . . . . .
S2 S -0.8506(5) 0.67955(15) 0.76933(12) 0.0440(7) Uani 1 1 d . . . . .
S3 S 0.5274(4) 0.35516(12) 0.75113(11) 0.0307(5) Uani 1 1 d . . . . .
S4 S 0.7363(5) 0.37726(16) 1.00176(11) 0.0482(7) Uani 1 1 d . . . . .
O1 O 0.2777(11) 0.3741(3) 0.6563(2) 0.0296(15) Uani 1 1 d . . . . .
B1 B 0.0999(18) 0.4030(6) 0.6266(4) 0.028(2) Uani 1 1 d . . . . .
C1 C -0.0382(17) 0.4529(5) 0.6631(4) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.0001(16) 0.4666(5) 0.7233(4) 0.027(2) Uani 1 1 d . . . . .
C3 C -0.1523(16) 0.5119(5) 0.7484(4) 0.032(2) Uani 1 1 d . . . . .
H3 H -0.149286 0.526532 0.788742 0.038 Uiso 1 1 calc R U . . .
C4 C -0.3067(15) 0.5334(5) 0.7095(4) 0.026(2) Uani 1 1 d . . . . .
C5 C -0.4845(17) 0.5794(5) 0.7220(4) 0.032(2) Uani 1 1 d . . . . .
H5 H -0.490064 0.599353 0.760731 0.039 Uiso 1 1 calc R U . . .
C6 C -0.6430(17) 0.5974(5) 0.6856(4) 0.030(2) Uani 1 1 d . . . . .
H6 H -0.640437 0.577014 0.646981 0.036 Uiso 1 1 calc R U . . .
C7 C -0.8174(15) 0.6448(5) 0.6993(4) 0.029(2) Uani 1 1 d . . . . .
C8 C -0.9760(15) 0.6685(5) 0.6596(4) 0.029(2) Uani 1 1 d . . . . .
H8 H -0.985353 0.656076 0.618817 0.035 Uiso 1 1 calc R U . . .
C9 C -1.121(2) 0.7145(6) 0.6912(5) 0.045(3) Uani 1 1 d . . . . .
H9 H -1.241542 0.735566 0.673178 0.054 Uiso 1 1 calc R U . . .
C10 C -1.0717(19) 0.7251(5) 0.7481(5) 0.044(3) Uani 1 1 d . . . . .
H10 H -1.151364 0.754861 0.774056 0.053 Uiso 1 1 calc R U . . .
C11 C 0.3132(16) 0.3902(5) 0.7142(4) 0.030(2) Uani 1 1 d . . . . .
C12 C 0.1856(15) 0.4328(4) 0.7489(4) 0.027(2) Uani 1 1 d . . . . .
C13 C 0.2670(17) 0.4368(5) 0.8073(4) 0.029(2) Uani 1 1 d . . . . .
H13 H 0.200836 0.463706 0.837943 0.035 Uiso 1 1 calc R U . . .
C14 C 0.4500(17) 0.3982(5) 0.8159(4) 0.032(2) Uani 1 1 d . . . . .
C15 C 0.5661(16) 0.3926(5) 0.8708(4) 0.033(2) Uani 1 1 d . . . . .
H15 H 0.502652 0.413884 0.904682 0.040 Uiso 1 1 calc R U . . .
C16 C 0.7523(18) 0.3608(5) 0.8793(4) 0.034(2) Uani 1 1 d . . . . .
H16 H 0.822990 0.342180 0.845496 0.041 Uiso 1 1 calc R U . . .
C17 C 0.8558(17) 0.3524(5) 0.9368(4) 0.033(2) Uani 1 1 d . . . . .
C18 C 1.0574(17) 0.3213(5) 0.9468(4) 0.034(2) Uani 1 1 d . . . . .
H18 H 1.150572 0.304987 0.916741 0.040 Uiso 1 1 calc R U . . .
C19 C 1.0985(19) 0.3183(6) 1.0091(5) 0.044(3) Uani 1 1 d . . . . .
H19 H 1.224280 0.298964 1.025409 0.052 Uiso 1 1 calc R U . . .
C20 C 0.9421(19) 0.3454(6) 1.0420(5) 0.043(3) Uani 1 1 d . . . . .
H20 H 0.945980 0.346779 1.084024 0.052 Uiso 1 1 calc R U . . .
C21 C 0.0505(16) 0.3806(5) 0.5613(4) 0.028(2) Uani 1 1 d . . . . .
C22 C -0.1135(17) 0.3305(5) 0.5509(4) 0.035(2) Uani 1 1 d . . . . .
C23 C -0.1844(18) 0.3171(6) 0.4938(4) 0.040(3) Uani 1 1 d . . . . .
H23 H -0.296220 0.283773 0.487781 0.047 Uiso 1 1 calc R U . . .
C24 C -0.095(2) 0.3514(6) 0.4455(5) 0.046(3) Uani 1 1 d . . . . .
C25 C 0.0713(19) 0.3986(6) 0.4553(4) 0.043(3) Uani 1 1 d . . . . .
H25 H 0.135106 0.421602 0.422219 0.051 Uiso 1 1 calc R U . . .
C26 C 0.1486(19) 0.4136(5) 0.5124(4) 0.039(3) Uani 1 1 d . . . . .
C27 C -0.221(2) 0.2918(6) 0.6016(4) 0.052(3) Uani 1 1 d . . . . .
H27A H -0.370151 0.305113 0.602512 0.078 Uiso 1 1 calc R U . . .
H27B H -0.154189 0.305640 0.639025 0.078 Uiso 1 1 calc R U . . .
H27C H -0.207847 0.239399 0.595974 0.078 Uiso 1 1 calc R U . . .
C28 C -0.172(2) 0.3372(8) 0.3834(5) 0.071(4) Uani 1 1 d . . . . .
H28A H -0.271693 0.296807 0.383811 0.107 Uiso 1 1 calc R U . . .
H28B H -0.052230 0.325142 0.357848 0.107 Uiso 1 1 calc R U . . .
H28C H -0.242220 0.380590 0.368102 0.107 Uiso 1 1 calc R U . . .
C29 C 0.326(3) 0.4664(8) 0.5211(6) 0.078(5) Uani 1 1 d . . . . .
H29A H 0.347854 0.493834 0.484488 0.117 Uiso 1 1 calc R U . . .
H29B H 0.454737 0.440000 0.531141 0.117 Uiso 1 1 calc R U . . .
H29C H 0.290208 0.499686 0.553330 0.117 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.726(10) . ?
S1 C4 1.728(9) . ?
S2 C10 1.706(11) . ?
S2 C7 1.719(9) . ?
S3 C11 1.722(10) . ?
S3 C14 1.736(10) . ?
S4 C20 1.697(12) . ?
S4 C17 1.713(10) . ?
O1 C11 1.359(10) . ?
O1 B1 1.418(13) . ?
B1 C1 1.516(14) . ?
B1 C21 1.563(12) . ?
C1 C2 1.402(12) . ?
C2 C3 1.401(13) . ?
C2 C12 1.453(13) . ?
C3 C4 1.375(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.441(13) . ?
C5 C6 1.342(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.446(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.419(13) . ?
C8 C9 1.444(14) . ?
C8 H8 0.9500 . ?
C9 C10 1.336(15) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.374(12) . ?
C12 C13 1.420(12) . ?
C13 C14 1.377(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.447(13) . ?
C15 C16 1.334(14) . ?
C15 H15 0.9500 . ?
C16 C17 1.464(13) . ?
C16 H16 0.9500 . ?
C17 C18 1.422(15) . ?
C18 C19 1.430(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.338(16) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.408(13) . ?
C21 C22 1.413(14) . ?
C22 C23 1.388(13) . ?
C22 C27 1.512(14) . ?
C23 C24 1.385(15) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(16) . ?
C24 C28 1.509(14) . ?
C25 C26 1.407(14) . ?
C25 H25 0.9500 . ?
C26 C29 1.502(17) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C4 92.5(4) . . ?
C10 S2 C7 91.6(5) . . ?
C11 S3 C14 90.6(5) . . ?
C20 S4 C17 91.3(5) . . ?
C11 O1 B1 120.3(8) . . ?
O1 B1 C1 115.6(8) . . ?
O1 B1 C21 120.4(9) . . ?
C1 B1 C21 123.9(9) . . ?
C2 C1 B1 122.4(9) . . ?
C2 C1 S1 110.5(7) . . ?
B1 C1 S1 127.1(7) . . ?
C3 C2 C1 112.4(9) . . ?
C3 C2 C12 131.0(8) . . ?
C1 C2 C12 116.6(8) . . ?
C4 C3 C2 114.0(8) . . ?
C4 C3 H3 123.0 . . ?
C2 C3 H3 123.0 . . ?
C3 C4 C5 127.2(8) . . ?
C3 C4 S1 110.7(7) . . ?
C5 C4 S1 122.2(7) . . ?
C6 C5 C4 127.9(9) . . ?
C6 C5 H5 116.0 . . ?
C4 C5 H5 116.0 . . ?
C5 C6 C7 126.5(8) . . ?
C5 C6 H6 116.8 . . ?
C7 C6 H6 116.8 . . ?
C8 C7 C6 126.6(8) . . ?
C8 C7 S2 112.3(7) . . ?
C6 C7 S2 121.2(7) . . ?
C7 C8 C9 108.8(9) . . ?
C7 C8 H8 125.6 . . ?
C9 C8 H8 125.6 . . ?
C10 C9 C8 114.3(11) . . ?
C10 C9 H9 122.8 . . ?
C8 C9 H9 122.8 . . ?
C9 C10 S2 113.0(9) . . ?
C9 C10 H10 123.5 . . ?
S2 C10 H10 123.5 . . ?
O1 C11 C12 125.1(9) . . ?
O1 C11 S3 120.9(7) . . ?
C12 C11 S3 114.0(7) . . ?
C11 C12 C13 110.1(9) . . ?
C11 C12 C2 119.9(8) . . ?
C13 C12 C2 130.0(8) . . ?
C14 C13 C12 114.2(8) . . ?
C14 C13 H13 122.9 . . ?
C12 C13 H13 122.9 . . ?
C13 C14 C15 126.0(9) . . ?
C13 C14 S3 111.0(7) . . ?
C15 C14 S3 123.0(8) . . ?
C16 C15 C14 127.4(9) . . ?
C16 C15 H15 116.3 . . ?
C14 C15 H15 116.3 . . ?
C15 C16 C17 124.9(9) . . ?
C15 C16 H16 117.6 . . ?
C17 C16 H16 117.6 . . ?
C18 C17 C16 126.0(9) . . ?
C18 C17 S4 111.8(7) . . ?
C16 C17 S4 122.1(8) . . ?
C17 C18 C19 109.6(10) . . ?
C17 C18 H18 125.2 . . ?
C19 C18 H18 125.2 . . ?
C20 C19 C18 113.3(10) . . ?
C20 C19 H19 123.4 . . ?
C18 C19 H19 123.4 . . ?
C19 C20 S4 113.9(8) . . ?
C19 C20 H20 123.1 . . ?
S4 C20 H20 123.1 . . ?
C26 C21 C22 118.7(9) . . ?
C26 C21 B1 122.4(9) . . ?
C22 C21 B1 118.6(9) . . ?
C23 C22 C21 120.7(10) . . ?
C23 C22 C27 118.1(10) . . ?
C21 C22 C27 121.2(9) . . ?
C24 C23 C22 121.1(10) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C25 118.4(9) . . ?
C23 C24 C28 121.2(11) . . ?
C25 C24 C28 120.3(11) . . ?
C24 C25 C26 122.4(10) . . ?
C24 C25 H25 118.8 . . ?
C26 C25 H25 118.8 . . ?
C25 C26 C21 118.6(10) . . ?
C25 C26 C29 120.7(10) . . ?
C21 C26 C29 120.7(9) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
C11 O1 B1 C1 1.3(12) . . . . ?
C11 O1 B1 C21 -176.0(8) . . . . ?
O1 B1 C1 C2 -3.3(14) . . . . ?
C21 B1 C1 C2 173.9(9) . . . . ?
O1 B1 C1 S1 179.9(7) . . . . ?
C21 B1 C1 S1 -2.9(14) . . . . ?
C4 S1 C1 C2 0.4(7) . . . . ?
C4 S1 C1 B1 177.5(9) . . . . ?
B1 C1 C2 C3 -177.7(9) . . . . ?
S1 C1 C2 C3 -0.4(10) . . . . ?
B1 C1 C2 C12 2.5(13) . . . . ?
S1 C1 C2 C12 179.7(6) . . . . ?
C1 C2 C3 C4 0.1(12) . . . . ?
C12 C2 C3 C4 180.0(9) . . . . ?
C2 C3 C4 C5 179.6(9) . . . . ?
C2 C3 C4 S1 0.2(10) . . . . ?
C1 S1 C4 C3 -0.4(7) . . . . ?
C1 S1 C4 C5 -179.8(8) . . . . ?
C3 C4 C5 C6 -175.7(10) . . . . ?
S1 C4 C5 C6 3.6(14) . . . . ?
C4 C5 C6 C7 -178.8(9) . . . . ?
C5 C6 C7 C8 174.6(9) . . . . ?
C5 C6 C7 S2 -5.0(13) . . . . ?
C10 S2 C7 C8 0.2(8) . . . . ?
C10 S2 C7 C6 179.9(8) . . . . ?
C6 C7 C8 C9 179.4(9) . . . . ?
S2 C7 C8 C9 -0.9(10) . . . . ?
C7 C8 C9 C10 1.4(13) . . . . ?
C8 C9 C10 S2 -1.2(13) . . . . ?
C7 S2 C10 C9 0.6(9) . . . . ?
B1 O1 C11 C12 1.4(13) . . . . ?
B1 O1 C11 S3 179.6(7) . . . . ?
C14 S3 C11 O1 -178.7(7) . . . . ?
C14 S3 C11 C12 -0.3(7) . . . . ?
O1 C11 C12 C13 178.5(8) . . . . ?
S3 C11 C12 C13 0.2(10) . . . . ?
O1 C11 C12 C2 -2.4(13) . . . . ?
S3 C11 C12 C2 179.3(7) . . . . ?
C3 C2 C12 C11 -179.6(10) . . . . ?
C1 C2 C12 C11 0.3(12) . . . . ?
C3 C2 C12 C13 -0.7(16) . . . . ?
C1 C2 C12 C13 179.2(9) . . . . ?
C11 C12 C13 C14 0.0(11) . . . . ?
C2 C12 C13 C14 -179.0(9) . . . . ?
C12 C13 C14 C15 -179.7(9) . . . . ?
C12 C13 C14 S3 -0.2(11) . . . . ?
C11 S3 C14 C13 0.3(7) . . . . ?
C11 S3 C14 C15 179.8(8) . . . . ?
C13 C14 C15 C16 -174.0(10) . . . . ?
S3 C14 C15 C16 6.6(15) . . . . ?
C14 C15 C16 C17 -175.6(9) . . . . ?
C15 C16 C17 C18 -177.4(10) . . . . ?
C15 C16 C17 S4 5.1(15) . . . . ?
C20 S4 C17 C18 -1.6(8) . . . . ?
C20 S4 C17 C16 176.2(9) . . . . ?
C16 C17 C18 C19 -176.2(10) . . . . ?
S4 C17 C18 C19 1.5(11) . . . . ?
C17 C18 C19 C20 -0.6(13) . . . . ?
C18 C19 C20 S4 -0.6(13) . . . . ?
C17 S4 C20 C19 1.3(9) . . . . ?
O1 B1 C21 C26 -83.0(12) . . . . ?
C1 B1 C21 C26 99.9(13) . . . . ?
O1 B1 C21 C22 103.4(11) . . . . ?
C1 B1 C21 C22 -73.7(12) . . . . ?
C26 C21 C22 C23 -3.5(15) . . . . ?
B1 C21 C22 C23 170.3(10) . . . . ?
C26 C21 C22 C27 178.3(10) . . . . ?
B1 C21 C22 C27 -7.9(15) . . . . ?
C21 C22 C23 C24 0.9(16) . . . . ?
C27 C22 C23 C24 179.3(11) . . . . ?
C22 C23 C24 C25 1.4(17) . . . . ?
C22 C23 C24 C28 -179.6(11) . . . . ?
C23 C24 C25 C26 -1.1(17) . . . . ?
C28 C24 C25 C26 179.9(11) . . . . ?
C24 C25 C26 C21 -1.4(17) . . . . ?
C24 C25 C26 C29 -178.7(12) . . . . ?
C22 C21 C26 C25 3.6(15) . . . . ?
B1 C21 C26 C25 -169.9(10) . . . . ?
C22 C21 C26 C29 -179.1(11) . . . . ?
B1 C21 C26 C29 7.3(17) . . . . ?

_refine_diff_density_max         0.390
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.094


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

data_8_wa3190_revised_by_AVirovets
_database_code_depnum_ccdc_archive 'CCDC 2384688'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT340_8_wa3190_revised_by_AVirovets 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01067 Ang.  
RESPONSE: The twinned crystal was scattering very weakly.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H8 O3 S2'
_chemical_formula_sum            'C11 H8 O3 S2'
_chemical_formula_weight         252.29

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   3.8781(3)
_cell_length_b                   8.6909(6)
_cell_length_c                   32.175(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.658(7)
_cell_angle_gamma                90
_cell_volume                     1083.99(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1178
_cell_measurement_theta_min      2.4540
_cell_measurement_theta_max      23.0070

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.477
_shelx_estimated_absorpt_T_min   0.958
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_T_min  0.01548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            2393
_diffrn_reflns_av_unetI/netI     0.2118
_diffrn_reflns_av_R_equivalents  0.2195
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.428
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2393
_reflns_number_gt                1158
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.

The non-overlapping reflections from the 2nd, minor component were removed
using HKLF5tools routine:
https://www.uni-marburg.de/en/fb15/researchgroups/ag-kraus/research/hklf5tools
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0784P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2393
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.0759
_refine_ls_wR_factor_ref         0.1816
_refine_ls_wR_factor_gt          0.1623
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_restrained_S_all      0.909
_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
S1 S 0.2274(6) 0.4848(2) 0.05149(6) 0.0285(6) Uani 1 1 d . . . . .
S2 S 0.9811(7) 0.9481(2) 0.18170(7) 0.0324(7) Uani 1 1 d . . . . .
O1 O 0.4231(17) 0.7806(6) 0.06216(16) 0.0341(17) Uani 1 1 d . . . . .
O2 O 0.067(2) 0.1405(7) 0.0642(2) 0.055(2) Uani 1 1 d . . . . .
O3 O 1.2156(19) 0.8763(7) 0.27313(17) 0.050(2) Uani 1 1 d . . . . .
C1 C 0.404(2) 0.6390(9) 0.0783(2) 0.025(2) Uani 1 1 d . . . . .
C2 C 0.547(2) 0.6000(9) 0.1170(2) 0.030(2) Uani 1 1 d . . . . .
C3 C 0.490(2) 0.4432(9) 0.1248(2) 0.029(2) Uani 1 1 d . . . . .
H3 H 0.564721 0.395000 0.149982 0.034 Uiso 1 1 calc R U . . .
C4 C 0.321(3) 0.3649(10) 0.0938(2) 0.030(2) Uani 1 1 d . . . . .
C5 C 0.232(3) 0.2050(10) 0.0921(3) 0.043(3) Uani 1 1 d . . . . .
H5 H 0.308060 0.142977 0.114903 0.051 Uiso 1 1 calc R U . . .
C6 C 0.247(2) 0.8073(10) 0.0217(2) 0.037(3) Uani 1 1 d . . . . .
H6A H 0.359227 0.746901 0.000269 0.056 Uiso 1 1 calc R U . . .
H6B H 0.258579 0.916880 0.014710 0.056 Uiso 1 1 calc R U . . .
H6C H 0.004647 0.775967 0.023266 0.056 Uiso 1 1 calc R U . . .
C11 C 0.792(2) 0.8596(9) 0.1392(2) 0.029(2) Uani 1 1 d . . . . .
H11 H 0.751030 0.908655 0.113124 0.035 Uiso 1 1 calc R U . . .
C12 C 0.707(2) 0.7102(9) 0.1473(2) 0.023(2) Uani 1 1 d . . . . .
C13 C 0.803(2) 0.6672(9) 0.1881(2) 0.030(2) Uani 1 1 d . . . . .
H13 H 0.771842 0.566224 0.198712 0.036 Uiso 1 1 calc R U . . .
C14 C 0.943(2) 0.7822(9) 0.2107(2) 0.024(2) Uani 1 1 d . . . . .
C15 C 1.075(3) 0.7738(11) 0.2534(2) 0.037(3) Uani 1 1 d . . . . .
H15 H 1.048997 0.678199 0.267261 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.724(8) . ?
S1 C4 1.745(8) . ?
S2 C11 1.715(8) . ?
S2 C14 1.725(8) . ?
O1 C1 1.339(9) . ?
O1 C6 1.471(9) . ?
O2 C5 1.223(10) . ?
O3 C15 1.214(9) . ?
C1 C2 1.391(11) . ?
C2 C3 1.404(10) . ?
C2 C12 1.489(10) . ?
C3 C4 1.360(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.433(12) . ?
C5 H5 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C11 C12 1.367(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.405(10) . ?
C13 C14 1.341(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.455(10) . ?
C15 H15 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C4 90.2(4) . . ?
C11 S2 C14 90.9(4) . . ?
C1 O1 C6 117.3(6) . . ?
O1 C1 C2 123.1(7) . . ?
O1 C1 S1 123.1(6) . . ?
C2 C1 S1 113.6(6) . . ?
C1 C2 C3 109.6(7) . . ?
C1 C2 C12 125.3(7) . . ?
C3 C2 C12 124.9(7) . . ?
C4 C3 C2 115.5(7) . . ?
C4 C3 H3 122.3 . . ?
C2 C3 H3 122.3 . . ?
C3 C4 C5 128.6(7) . . ?
C3 C4 S1 111.0(6) . . ?
C5 C4 S1 120.4(6) . . ?
O2 C5 C4 126.4(8) . . ?
O2 C5 H5 116.8 . . ?
C4 C5 H5 116.8 . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C12 C11 S2 111.9(6) . . ?
C12 C11 H11 124.0 . . ?
S2 C11 H11 124.0 . . ?
C11 C12 C13 111.9(7) . . ?
C11 C12 C2 125.8(7) . . ?
C13 C12 C2 122.3(7) . . ?
C14 C13 C12 113.5(7) . . ?
C14 C13 H13 123.2 . . ?
C12 C13 H13 123.2 . . ?
C13 C14 C15 126.9(8) . . ?
C13 C14 S2 111.8(6) . . ?
C15 C14 S2 121.2(6) . . ?
O3 C15 C14 126.7(8) . . ?
O3 C15 H15 116.6 . . ?
C14 C15 H15 116.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 O1 C1 C2 -177.2(9) . . . . ?
C6 O1 C1 S1 7.6(11) . . . . ?
C4 S1 C1 O1 178.9(8) . . . . ?
C4 S1 C1 C2 3.3(8) . . . . ?
O1 C1 C2 C3 -178.8(8) . . . . ?
S1 C1 C2 C3 -3.2(11) . . . . ?
O1 C1 C2 C12 6.3(15) . . . . ?
S1 C1 C2 C12 -178.1(7) . . . . ?
C1 C2 C3 C4 1.3(13) . . . . ?
C12 C2 C3 C4 176.2(9) . . . . ?
C2 C3 C4 C5 178.8(10) . . . . ?
C2 C3 C4 S1 1.2(11) . . . . ?
C1 S1 C4 C3 -2.5(8) . . . . ?
C1 S1 C4 C5 179.7(9) . . . . ?
C3 C4 C5 O2 176.8(11) . . . . ?
S1 C4 C5 O2 -5.8(15) . . . . ?
C14 S2 C11 C12 -0.3(8) . . . . ?
S2 C11 C12 C13 -1.1(10) . . . . ?
S2 C11 C12 C2 -178.6(7) . . . . ?
C1 C2 C12 C11 -12.0(15) . . . . ?
C3 C2 C12 C11 173.9(10) . . . . ?
C1 C2 C12 C13 170.9(10) . . . . ?
C3 C2 C12 C13 -3.3(14) . . . . ?
C11 C12 C13 C14 2.6(12) . . . . ?
C2 C12 C13 C14 -179.9(8) . . . . ?
C12 C13 C14 C15 -178.4(9) . . . . ?
C12 C13 C14 S2 -2.8(11) . . . . ?
C11 S2 C14 C13 1.8(8) . . . . ?
C11 S2 C14 C15 177.7(8) . . . . ?
C13 C14 C15 O3 176.4(10) . . . . ?
S2 C14 C15 O3 1.2(15) . . . . ?

_refine_diff_density_max         0.424
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.098


####################################################################### 
# 
# 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_6_wa3333
_database_code_depnum_ccdc_archive 'CCDC 2384686'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT213_6_wa3333            
;
PROBLEM: Atom C18             has ADP max/min Ratio .....        3.2 prolat
RESPONSE: The whole Mes group suffers from a positional disorder over two
very close positions against B1-C11 bond. This disorder is approximated with 
the elongated a.d.p. ellipsoids.
;
_vrf_PLAT220_6_wa3333            
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        4.8 Ratio 
RESPONSE: The whole Mes group suffers from a positional disorder over two
very close positions against B1-C11 bond. This disorder is approximated with 
the elongated a.d.p. ellipsoids.
;
_vrf_PLAT222_6_wa3333            
;
PROBLEM: NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        5.5 Ratio 
RESPONSE: The whole Mes group suffers from a positional disorder over two
very close positions against B1-C11 bond. This disorder is approximated with 
the elongated a.d.p. ellipsoids.
;
_vrf_PLAT230_6_wa3333            
;
PROBLEM: Hirshfeld Test Diff for    C13      --C14      .        6.0 s.u.  
RESPONSE: The whole Mes group suffers from a positional disorder over two
very close positions against B1-C11 bond. This disorder is approximated with 
the elongated a.d.p. ellipsoids.
;
_vrf_PLAT910_6_wa3333            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          9 Note  
RESPONSE: These reflections are hidden by the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H30 B2 O2 S4'
_chemical_formula_sum            'C36 H30 B2 O2 S4'
_chemical_formula_weight         644.46

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'
B B 0.0013 0.0007 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   12.7041(5)
_cell_length_b                   6.2990(3)
_cell_length_c                   20.8628(11)
_cell_angle_alpha                90
_cell_angle_beta                 99.828(4)
_cell_angle_gamma                90
_cell_volume                     1645.01(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3386
_cell_measurement_theta_min      4.0100
_cell_measurement_theta_max      28.7590

_exptl_crystal_description       plank
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.321
_shelx_estimated_absorpt_T_min   0.843
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_T_min  0.08089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            11399
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.794
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3352
_reflns_number_gt                2506
_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       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0580P)²+0.1101P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3352
_refine_ls_number_parameters     202
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1045
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
B1 B 0.72729(18) 0.3734(4) 0.36221(12) 0.0286(5) Uani 1 1 d . . . . .
S1 S 0.82523(4) 0.72410(8) 0.44155(3) 0.02892(16) Uani 1 1 d . . . . .
S2 S 0.88048(4) -0.07188(9) 0.27851(3) 0.03456(18) Uani 1 1 d . . . . .
O1 O 0.74968(11) 0.1979(2) 0.32562(7) 0.0304(4) Uani 1 1 d . . . . .
C1 C 0.82428(15) 0.4954(3) 0.39579(10) 0.0262(5) Uani 1 1 d . . . . .
C2 C 0.92814(15) 0.4393(3) 0.38930(10) 0.0244(4) Uani 1 1 d . . . . .
C3 C 1.00593(15) 0.5828(3) 0.42053(10) 0.0264(5) Uani 1 1 d . . . . .
H3 H 1.080315 0.567300 0.420542 0.032 Uiso 1 1 calc R U . . .
C4 C 0.96312(15) 0.7461(3) 0.45071(10) 0.0261(5) Uani 1 1 d . . . . .
C5 C 1.02154(16) 0.9188(3) 0.48616(10) 0.0288(5) Uani 1 1 d . . . . .
H5 H 1.097143 0.916612 0.490104 0.035 Uiso 1 1 calc R U . . .
C6 C 0.85195(16) 0.1462(3) 0.32257(11) 0.0278(5) Uani 1 1 d . . . . .
C7 C 0.94143(15) 0.2523(3) 0.35195(10) 0.0252(5) Uani 1 1 d . . . . .
C8 C 1.03624(16) 0.1502(3) 0.33856(11) 0.0294(5) Uani 1 1 d . . . . .
H8 H 1.106432 0.198913 0.354989 0.035 Uiso 1 1 calc R U . . .
C9 C 1.01533(17) -0.0218(4) 0.30029(11) 0.0334(5) Uani 1 1 d . . . . .
H9 H 1.069216 -0.106877 0.286688 0.040 Uiso 1 1 calc R U . . .
C11 C 0.60799(16) 0.4300(3) 0.36518(12) 0.0336(5) Uani 1 1 d . . . . .
C12 C 0.55753(17) 0.5979(4) 0.32831(14) 0.0442(7) Uani 1 1 d . . . . .
C13 C 0.4544(2) 0.6570(5) 0.33629(18) 0.0626(9) Uani 1 1 d . . . . .
H13 H 0.419925 0.771053 0.311275 0.075 Uiso 1 1 calc R U . . .
C14 C 0.40124(19) 0.5526(6) 0.37994(18) 0.0673(10) Uani 1 1 d . . . . .
C15 C 0.4516(2) 0.3880(6) 0.41577(16) 0.0645(9) Uani 1 1 d . . . . .
H15 H 0.415971 0.316995 0.446090 0.077 Uiso 1 1 calc R U . . .
C16 C 0.55370(18) 0.3223(5) 0.40879(13) 0.0466(7) Uani 1 1 d . . . . .
C17 C 0.6115(2) 0.7117(5) 0.27941(17) 0.0651(9) Uani 1 1 d . . . . .
H17A H 0.628744 0.857109 0.294301 0.098 Uiso 1 1 calc R U . . .
H17B H 0.563575 0.715309 0.237306 0.098 Uiso 1 1 calc R U . . .
H17C H 0.677400 0.636736 0.274769 0.098 Uiso 1 1 calc R U . . .
C18 C 0.2897(2) 0.6226(8) 0.3878(2) 0.1164(19) Uani 1 1 d . . . . .
H18A H 0.236762 0.550505 0.355401 0.175 Uiso 1 1 calc R U . . .
H18B H 0.283034 0.776543 0.381556 0.175 Uiso 1 1 calc R U . . .
H18C H 0.277286 0.585981 0.431572 0.175 Uiso 1 1 calc R U . . .
C19 C 0.6041(2) 0.1354(5) 0.44794(16) 0.0649(9) Uani 1 1 d . . . . .
H19A H 0.577178 0.127741 0.489180 0.097 Uiso 1 1 calc R U . . .
H19B H 0.681910 0.153158 0.456749 0.097 Uiso 1 1 calc R U . . .
H19C H 0.586033 0.004209 0.423281 0.097 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
B1 O1 1.400(3) . ?
B1 C1 1.518(3) . ?
B1 C11 1.568(3) . ?
S1 C1 1.727(2) . ?
S1 C4 1.735(2) . ?
S2 C9 1.725(2) . ?
S2 C6 1.725(2) . ?
O1 C6 1.352(2) . ?
C1 C2 1.395(3) . ?
C2 C3 1.414(3) . ?
C2 C7 1.438(3) . ?
C3 C4 1.366(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.447(3) . ?
C5 C5 1.337(4) 3_776 ?
C5 H5 0.9500 . ?
C6 C7 1.370(3) . ?
C7 C8 1.434(3) . ?
C8 C9 1.345(3) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C11 C12 1.398(3) . ?
C11 C16 1.406(4) . ?
C12 C13 1.399(4) . ?
C12 C17 1.505(4) . ?
C13 C14 1.388(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.371(5) . ?
C14 C18 1.520(4) . ?
C15 C16 1.393(4) . ?
C15 H15 0.9500 . ?
C16 C19 1.512(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 B1 C1 115.26(19) . . ?
O1 B1 C11 119.24(18) . . ?
C1 B1 C11 125.5(2) . . ?
C1 S1 C4 92.24(10) . . ?
C9 S2 C6 90.20(10) . . ?
C6 O1 B1 120.17(16) . . ?
C2 C1 B1 122.28(19) . . ?
C2 C1 S1 110.33(14) . . ?
B1 C1 S1 127.28(16) . . ?
C1 C2 C3 113.07(18) . . ?
C1 C2 C7 117.42(17) . . ?
C3 C2 C7 129.49(18) . . ?
C4 C3 C2 113.06(17) . . ?
C4 C3 H3 123.5 . . ?
C2 C3 H3 123.5 . . ?
C3 C4 C5 126.27(19) . . ?
C3 C4 S1 111.28(15) . . ?
C5 C4 S1 122.44(16) . . ?
C5 C5 C4 125.7(2) 3_776 . ?
C5 C5 H5 117.1 3_776 . ?
C4 C5 H5 117.1 . . ?
O1 C6 C7 126.31(19) . . ?
O1 C6 S2 120.54(15) . . ?
C7 C6 S2 113.15(16) . . ?
C6 C7 C8 110.75(18) . . ?
C6 C7 C2 118.48(18) . . ?
C8 C7 C2 130.76(18) . . ?
C9 C8 C7 112.92(18) . . ?
C9 C8 H8 123.5 . . ?
C7 C8 H8 123.5 . . ?
C8 C9 S2 112.97(17) . . ?
C8 C9 H9 123.5 . . ?
S2 C9 H9 123.5 . . ?
C12 C11 C16 119.4(2) . . ?
C12 C11 B1 120.4(2) . . ?
C16 C11 B1 120.0(2) . . ?
C11 C12 C13 119.1(3) . . ?
C11 C12 C17 121.0(2) . . ?
C13 C12 C17 119.9(3) . . ?
C14 C13 C12 121.5(3) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C15 C14 C13 118.8(3) . . ?
C15 C14 C18 121.2(4) . . ?
C13 C14 C18 120.0(4) . . ?
C14 C15 C16 121.6(3) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C15 C16 C11 119.5(3) . . ?
C15 C16 C19 119.4(3) . . ?
C11 C16 C19 121.0(2) . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C14 C18 H18A 109.5 . . ?
C14 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C14 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
C1 B1 O1 C6 0.7(3) . . . . ?
C11 B1 O1 C6 -179.8(2) . . . . ?
O1 B1 C1 C2 1.5(3) . . . . ?
C11 B1 C1 C2 -178.0(2) . . . . ?
O1 B1 C1 S1 177.10(16) . . . . ?
C11 B1 C1 S1 -2.4(3) . . . . ?
C4 S1 C1 C2 0.87(16) . . . . ?
C4 S1 C1 B1 -175.2(2) . . . . ?
B1 C1 C2 C3 175.53(19) . . . . ?
S1 C1 C2 C3 -0.8(2) . . . . ?
B1 C1 C2 C7 -3.3(3) . . . . ?
S1 C1 C2 C7 -179.55(15) . . . . ?
C1 C2 C3 C4 0.2(3) . . . . ?
C7 C2 C3 C4 178.8(2) . . . . ?
C2 C3 C4 C5 -179.40(19) . . . . ?
C2 C3 C4 S1 0.5(2) . . . . ?
C1 S1 C4 C3 -0.78(17) . . . . ?
C1 S1 C4 C5 179.11(18) . . . . ?
C3 C4 C5 C5 177.9(3) . . . 3_776 ?
S1 C4 C5 C5 -2.0(4) . . . 3_776 ?
B1 O1 C6 C7 -0.9(3) . . . . ?
B1 O1 C6 S2 179.11(16) . . . . ?
C9 S2 C6 O1 -179.60(18) . . . . ?
C9 S2 C6 C7 0.46(17) . . . . ?
O1 C6 C7 C8 179.3(2) . . . . ?
S2 C6 C7 C8 -0.7(2) . . . . ?
O1 C6 C7 C2 -0.9(3) . . . . ?
S2 C6 C7 C2 179.01(15) . . . . ?
C1 C2 C7 C6 3.0(3) . . . . ?
C3 C2 C7 C6 -175.6(2) . . . . ?
C1 C2 C7 C8 -177.4(2) . . . . ?
C3 C2 C7 C8 4.1(4) . . . . ?
C6 C7 C8 C9 0.7(3) . . . . ?
C2 C7 C8 C9 -179.0(2) . . . . ?
C7 C8 C9 S2 -0.3(2) . . . . ?
C6 S2 C9 C8 -0.05(18) . . . . ?
O1 B1 C11 C12 -102.8(3) . . . . ?
C1 B1 C11 C12 76.6(3) . . . . ?
O1 B1 C11 C16 82.1(3) . . . . ?
C1 B1 C11 C16 -98.5(3) . . . . ?
C16 C11 C12 C13 0.8(3) . . . . ?
B1 C11 C12 C13 -174.3(2) . . . . ?
C16 C11 C12 C17 -177.8(2) . . . . ?
B1 C11 C12 C17 7.1(3) . . . . ?
C11 C12 C13 C14 0.0(4) . . . . ?
C17 C12 C13 C14 178.6(3) . . . . ?
C12 C13 C14 C15 -0.1(4) . . . . ?
C12 C13 C14 C18 179.4(3) . . . . ?
C13 C14 C15 C16 -0.7(4) . . . . ?
C18 C14 C15 C16 179.8(3) . . . . ?
C14 C15 C16 C11 1.5(4) . . . . ?
C14 C15 C16 C19 -178.1(3) . . . . ?
C12 C11 C16 C15 -1.6(4) . . . . ?
B1 C11 C16 C15 173.6(2) . . . . ?
C12 C11 C16 C19 178.0(2) . . . . ?
B1 C11 C16 C19 -6.8(4) . . . . ?

_refine_diff_density_max         0.437
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.057


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

data_11_wa3185_revised_by_AVirovets
_database_code_depnum_ccdc_archive 'CCDC 2384691'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_RINTA01_11_wa3185_revised_by_AVirovets 
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: The crystal is twinned with the diffraction spots
from 2 domains significantly overlapping.
;
_vrf_PLAT410_11_wa3185_revised_by_AVirovets 
;
PROBLEM: Short Intra H...H Contact  H3       ..H19      .       1.89 Ang.  
RESPONSE: Both C atoms have sp2 hybridization, and there are no
signs for any other element (O, N etc.) in the corresponding
positions. Such contact can be caused by low quality of the
diffraction data.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C29 H21 B O S4'
_chemical_formula_sum            'C29 H21 B O S4'
_chemical_formula_weight         524.51

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'
B B 0.0013 0.0007 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   6.3634(6)
_cell_length_b                   15.1793(12)
_cell_length_c                   26.884(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.709(10)
_cell_angle_gamma                90
_cell_volume                     2588.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3797
_cell_measurement_theta_min      2.7120
_cell_measurement_theta_max      25.6190

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5989 16991 24966 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4011 16998 24966 nmt -1.0007 -0.0002 -0.0085 0.0003 0.9985 -0.0218 0.1675
-0.0755 -0.9962
_oxdiff_twin_integration_method  simultaneous
_twin_special_details            
;
Component 2 rotated by -177.7285° 
around [0.00 1.00 -0.04] (reciprocal) or [-0.00 1.00 -0.01] (direct)
;

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             1088
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.389
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_T_min  0.65751
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            8910
_diffrn_reflns_av_unetI/netI     0.2192
_diffrn_reflns_av_R_equivalents  0.2850
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.646
_diffrn_reflns_theta_max         25.680
_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             8910
_reflns_number_gt                4064
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.

The non-overlapping reflections from the 2nd, minor component were removed
using HKLF5tools routine:
https://www.uni-marburg.de/en/fb15/researchgroups/ag-kraus/research/hklf5tools
;

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          'Refined as a 2-component twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0873P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8910
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.1867
_refine_ls_wR_factor_gt          0.1634
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_restrained_S_all      0.902
_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
S1 S 0.6485(3) 0.42425(11) 0.60164(6) 0.0309(5) Uani 1 1 d . . . . .
S3 S -0.0763(3) 0.31183(10) 0.72550(7) 0.0299(5) Uani 1 1 d . . . . .
S4 S -0.0383(4) -0.03561(14) 0.60947(9) 0.0713(8) Uani 1 1 d . . . . .
O1 O 0.1834(6) 0.4322(2) 0.69644(15) 0.0259(11) Uani 1 1 d . . . . .
B1 B 0.3362(11) 0.4677(5) 0.6681(3) 0.0226(17) Uani 1 1 d . . . . .
C1 C 0.4364(9) 0.4022(4) 0.6357(2) 0.0231(16) Uani 1 1 d . . . . .
C2 C 0.3856(9) 0.3128(4) 0.6341(2) 0.0216(14) Uani 1 1 d . . . . .
C3 C 0.5294(10) 0.2635(4) 0.6064(2) 0.0268(16) Uani 1 1 d . . . . .
H3 H 0.523044 0.201339 0.602474 0.032 Uiso 1 1 calc R U . . .
C4 C 0.6772(9) 0.3156(4) 0.5862(2) 0.0301(16) Uani 1 1 d . . . . .
C5 C 0.8365(10) 0.2860(4) 0.5546(2) 0.0345(18) Uani 1 1 d . . . . .
H5 H 0.837643 0.225702 0.545201 0.041 Uiso 1 1 calc R U . . .
C6 C 0.9859(11) 0.3409(5) 0.5378(2) 0.0394(19) Uani 1 1 d . . . . .
H6 H 0.985549 0.400073 0.549332 0.047 Uiso 1 1 calc R U . . .
C7 C 1.1434(11) 0.3186(5) 0.5044(2) 0.0382(18) Uani 1 1 d . . . . .
S2 S 1.1562(4) 0.21781(15) 0.47563(8) 0.0680(8) Uani 1 1 d . . . . .
C8 C 1.3040(9) 0.3760(5) 0.4899(2) 0.0303(17) Uani 1 1 d . . . . .
H8 H 1.324977 0.435111 0.500709 0.036 Uiso 1 1 calc R U . . .
C9 C 1.4292(12) 0.3302(6) 0.4562(3) 0.063(3) Uani 1 1 d . . . . .
H9 H 1.545599 0.356778 0.442047 0.075 Uiso 1 1 calc R U . . .
C10 C 1.3690(13) 0.2467(6) 0.4461(3) 0.065(3) Uani 1 1 d . . . . .
H10 H 1.438620 0.208460 0.424855 0.078 Uiso 1 1 calc R U . . .
C11 C 0.1244(9) 0.3472(4) 0.6909(2) 0.0234(16) Uani 1 1 d . . . . .
C12 C 0.2063(9) 0.2845(4) 0.6609(2) 0.0228(15) Uani 1 1 d . . . . .
C13 C 0.0859(9) 0.2025(4) 0.6635(2) 0.0243(15) Uani 1 1 d . . . . .
C14 C -0.0642(10) 0.2090(4) 0.6980(2) 0.0267(16) Uani 1 1 d . . . . .
C15 C -0.2033(10) 0.1414(4) 0.7090(3) 0.0327(17) Uani 1 1 d . . . . .
H15 H -0.301045 0.149768 0.733503 0.039 Uiso 1 1 calc R U . . .
C16 C -0.1956(11) 0.0641(5) 0.6842(3) 0.0407(19) Uani 1 1 d . . . . .
H16 H -0.284500 0.016467 0.691702 0.049 Uiso 1 1 calc R U . . .
C17 C -0.0554(12) 0.0557(4) 0.6475(3) 0.043(2) Uani 1 1 d . . . . .
C18 C 0.0842(11) 0.1236(4) 0.6352(2) 0.0358(18) Uani 1 1 d . . . . .
C19 C 0.1894(12) 0.0984(5) 0.5924(3) 0.056(2) Uani 1 1 d . . . . .
H19 H 0.285181 0.135957 0.577321 0.068 Uiso 1 1 calc R U . . .
C20 C 0.1407(14) 0.0161(5) 0.5753(3) 0.071(3) Uani 1 1 d . . . . .
H20 H 0.199435 -0.009778 0.547365 0.085 Uiso 1 1 calc R U . . .
C21 C 0.3839(10) 0.5686(4) 0.6737(2) 0.0234(15) Uani 1 1 d . . . . .
C22 C 0.2407(10) 0.6302(4) 0.6512(2) 0.0253(16) Uani 1 1 d . . . . .
C23 C 0.2841(10) 0.7204(4) 0.6559(2) 0.0267(16) Uani 1 1 d . . . . .
H23 H 0.186206 0.761740 0.640918 0.032 Uiso 1 1 calc R U . . .
C24 C 0.4656(11) 0.7502(4) 0.6816(3) 0.0319(18) Uani 1 1 d . . . . .
C25 C 0.6050(10) 0.6895(4) 0.7039(2) 0.0326(17) Uani 1 1 d . . . . .
H25 H 0.730826 0.709755 0.721706 0.039 Uiso 1 1 calc R U . . .
C26 C 0.5656(10) 0.5990(4) 0.7008(2) 0.0245(16) Uani 1 1 d . . . . .
C27 C 0.0448(10) 0.6004(4) 0.6206(3) 0.0404(19) Uani 1 1 d . . . . .
H27A H -0.038206 0.562114 0.640836 0.061 Uiso 1 1 calc R U . . .
H27B H 0.084586 0.567725 0.591314 0.061 Uiso 1 1 calc R U . . .
H27C H -0.039596 0.651875 0.609586 0.061 Uiso 1 1 calc R U . . .
C28 C 0.5148(12) 0.8477(4) 0.6859(3) 0.047(2) Uani 1 1 d . . . . .
H28A H 0.388935 0.881793 0.674681 0.070 Uiso 1 1 calc R U . . .
H28B H 0.629337 0.862139 0.665061 0.070 Uiso 1 1 calc R U . . .
H28C H 0.557979 0.862321 0.720772 0.070 Uiso 1 1 calc R U . . .
C29 C 0.7178(10) 0.5369(4) 0.7285(3) 0.0387(19) Uani 1 1 d . . . . .
H29A H 0.862204 0.558150 0.726352 0.058 Uiso 1 1 calc R U . . .
H29B H 0.703363 0.478067 0.713522 0.058 Uiso 1 1 calc R U . . .
H29C H 0.687030 0.533905 0.763550 0.058 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C4 1.714(7) . ?
S1 C1 1.725(5) . ?
S3 C11 1.726(6) . ?
S3 C14 1.731(6) . ?
S4 C20 1.713(7) . ?
S4 C17 1.732(7) . ?
O1 C11 1.349(6) . ?
O1 B1 1.393(7) . ?
B1 C1 1.497(9) . ?
B1 C21 1.567(9) . ?
C1 C2 1.396(8) . ?
C2 C3 1.436(8) . ?
C2 C12 1.463(7) . ?
C3 C4 1.375(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.445(8) . ?
C5 C6 1.370(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.439(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.421(9) . ?
C7 S2 1.720(7) . ?
S2 C10 1.683(8) . ?
C8 C9 1.434(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.345(11) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.377(7) . ?
C12 C13 1.466(8) . ?
C13 C14 1.390(8) . ?
C13 C18 1.417(8) . ?
C14 C15 1.402(8) . ?
C15 C16 1.353(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.418(8) . ?
C18 C19 1.430(9) . ?
C19 C20 1.358(9) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.393(8) . ?
C21 C22 1.407(8) . ?
C22 C23 1.401(8) . ?
C22 C27 1.506(9) . ?
C23 C24 1.374(9) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(9) . ?
C24 C28 1.516(8) . ?
C25 C26 1.398(8) . ?
C25 H25 0.9500 . ?
C26 C29 1.505(8) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 S1 C1 92.6(3) . . ?
C11 S3 C14 89.4(3) . . ?
C20 S4 C17 91.6(3) . . ?
C11 O1 B1 120.7(5) . . ?
O1 B1 C1 114.3(5) . . ?
O1 B1 C21 117.6(5) . . ?
C1 B1 C21 128.1(5) . . ?
C2 C1 B1 123.7(5) . . ?
C2 C1 S1 111.2(4) . . ?
B1 C1 S1 124.7(5) . . ?
C1 C2 C3 111.5(5) . . ?
C1 C2 C12 117.3(5) . . ?
C3 C2 C12 131.2(5) . . ?
C4 C3 C2 113.0(6) . . ?
C4 C3 H3 123.5 . . ?
C2 C3 H3 123.5 . . ?
C3 C4 C5 126.1(6) . . ?
C3 C4 S1 111.6(5) . . ?
C5 C4 S1 122.4(5) . . ?
C6 C5 C4 123.0(6) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C5 C6 C7 126.9(7) . . ?
C5 C6 H6 116.5 . . ?
C7 C6 H6 116.5 . . ?
C8 C7 C6 125.5(6) . . ?
C8 C7 S2 111.0(5) . . ?
C6 C7 S2 123.4(5) . . ?
C10 S2 C7 92.9(4) . . ?
C7 C8 C9 109.1(7) . . ?
C7 C8 H8 125.5 . . ?
C9 C8 H8 125.5 . . ?
C10 C9 C8 114.8(7) . . ?
C10 C9 H9 122.6 . . ?
C8 C9 H9 122.6 . . ?
C9 C10 S2 112.2(6) . . ?
C9 C10 H10 123.9 . . ?
S2 C10 H10 123.9 . . ?
O1 C11 C12 127.6(5) . . ?
O1 C11 S3 116.7(4) . . ?
C12 C11 S3 115.7(4) . . ?
C11 C12 C2 115.7(5) . . ?
C11 C12 C13 109.5(5) . . ?
C2 C12 C13 134.7(5) . . ?
C14 C13 C18 116.2(6) . . ?
C14 C13 C12 111.2(5) . . ?
C18 C13 C12 132.3(6) . . ?
C13 C14 C15 124.7(6) . . ?
C13 C14 S3 114.0(4) . . ?
C15 C14 S3 121.2(5) . . ?
C16 C15 C14 118.8(6) . . ?
C16 C15 H15 120.6 . . ?
C14 C15 H15 120.6 . . ?
C15 C16 C17 118.8(6) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
C16 C17 C18 123.4(6) . . ?
C16 C17 S4 124.6(5) . . ?
C18 C17 S4 111.9(5) . . ?
C13 C18 C17 117.8(6) . . ?
C13 C18 C19 132.3(6) . . ?
C17 C18 C19 109.7(6) . . ?
C20 C19 C18 114.3(7) . . ?
C20 C19 H19 122.9 . . ?
C18 C19 H19 122.9 . . ?
C19 C20 S4 112.5(6) . . ?
C19 C20 H20 123.8 . . ?
S4 C20 H20 123.8 . . ?
C26 C21 C22 119.1(6) . . ?
C26 C21 B1 121.4(6) . . ?
C22 C21 B1 119.6(6) . . ?
C23 C22 C21 119.6(6) . . ?
C23 C22 C27 119.4(6) . . ?
C21 C22 C27 120.9(6) . . ?
C24 C23 C22 121.2(6) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 118.8(6) . . ?
C23 C24 C28 121.3(6) . . ?
C25 C24 C28 119.8(7) . . ?
C24 C25 C26 121.6(6) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C21 C26 C25 119.6(6) . . ?
C21 C26 C29 121.6(6) . . ?
C25 C26 C29 118.8(6) . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28A 109.5 . . ?
C24 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C24 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 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
C11 O1 B1 C1 -4.9(9) . . . . ?
C11 O1 B1 C21 175.5(6) . . . . ?
O1 B1 C1 C2 -1.0(9) . . . . ?
C21 B1 C1 C2 178.6(6) . . . . ?
O1 B1 C1 S1 -172.9(4) . . . . ?
C21 B1 C1 S1 6.7(10) . . . . ?
C4 S1 C1 C2 -1.4(5) . . . . ?
C4 S1 C1 B1 171.4(6) . . . . ?
B1 C1 C2 C3 -170.4(6) . . . . ?
S1 C1 C2 C3 2.5(7) . . . . ?
B1 C1 C2 C12 8.0(9) . . . . ?
S1 C1 C2 C12 -179.2(5) . . . . ?
C1 C2 C3 C4 -2.6(8) . . . . ?
C12 C2 C3 C4 179.4(6) . . . . ?
C2 C3 C4 C5 -177.1(6) . . . . ?
C2 C3 C4 S1 1.5(8) . . . . ?
C1 S1 C4 C3 -0.1(5) . . . . ?
C1 S1 C4 C5 178.6(6) . . . . ?
C3 C4 C5 C6 -176.6(7) . . . . ?
S1 C4 C5 C6 5.0(10) . . . . ?
C4 C5 C6 C7 -176.7(6) . . . . ?
C5 C6 C7 C8 -176.2(7) . . . . ?
C5 C6 C7 S2 5.4(11) . . . . ?
C8 C7 S2 C10 1.4(6) . . . . ?
C6 C7 S2 C10 -180.0(6) . . . . ?
C6 C7 C8 C9 -179.7(7) . . . . ?
S2 C7 C8 C9 -1.1(7) . . . . ?
C7 C8 C9 C10 0.2(10) . . . . ?
C8 C9 C10 S2 0.9(10) . . . . ?
C7 S2 C10 C9 -1.3(7) . . . . ?
B1 O1 C11 C12 3.7(10) . . . . ?
B1 O1 C11 S3 -176.6(5) . . . . ?
C14 S3 C11 O1 177.9(5) . . . . ?
C14 S3 C11 C12 -2.3(5) . . . . ?
O1 C11 C12 C2 3.6(10) . . . . ?
S3 C11 C12 C2 -176.1(5) . . . . ?
O1 C11 C12 C13 -175.9(6) . . . . ?
S3 C11 C12 C13 4.4(7) . . . . ?
C1 C2 C12 C11 -9.0(8) . . . . ?
C3 C2 C12 C11 169.0(6) . . . . ?
C1 C2 C12 C13 170.4(7) . . . . ?
C3 C2 C12 C13 -11.6(12) . . . . ?
C11 C12 C13 C14 -4.7(8) . . . . ?
C2 C12 C13 C14 175.9(7) . . . . ?
C11 C12 C13 C18 169.7(7) . . . . ?
C2 C12 C13 C18 -9.7(13) . . . . ?
C18 C13 C14 C15 4.9(10) . . . . ?
C12 C13 C14 C15 -179.8(6) . . . . ?
C18 C13 C14 S3 -172.2(5) . . . . ?
C12 C13 C14 S3 3.1(7) . . . . ?
C11 S3 C14 C13 -0.6(5) . . . . ?
C11 S3 C14 C15 -177.8(6) . . . . ?
C13 C14 C15 C16 -1.0(11) . . . . ?
S3 C14 C15 C16 175.9(5) . . . . ?
C14 C15 C16 C17 -2.2(11) . . . . ?
C15 C16 C17 C18 1.3(12) . . . . ?
C15 C16 C17 S4 -175.4(6) . . . . ?
C20 S4 C17 C16 174.1(7) . . . . ?
C20 S4 C17 C18 -2.9(7) . . . . ?
C14 C13 C18 C17 -5.5(9) . . . . ?
C12 C13 C18 C17 -179.6(7) . . . . ?
C14 C13 C18 C19 169.5(8) . . . . ?
C12 C13 C18 C19 -4.6(13) . . . . ?
C16 C17 C18 C13 2.8(11) . . . . ?
S4 C17 C18 C13 179.8(5) . . . . ?
C16 C17 C18 C19 -173.3(7) . . . . ?
S4 C17 C18 C19 3.7(8) . . . . ?
C13 C18 C19 C20 -178.2(8) . . . . ?
C17 C18 C19 C20 -2.8(10) . . . . ?
C18 C19 C20 S4 0.7(11) . . . . ?
C17 S4 C20 C19 1.3(8) . . . . ?
O1 B1 C21 C26 104.4(7) . . . . ?
C1 B1 C21 C26 -75.1(9) . . . . ?
O1 B1 C21 C22 -75.5(8) . . . . ?
C1 B1 C21 C22 105.0(8) . . . . ?
C26 C21 C22 C23 0.7(8) . . . . ?
B1 C21 C22 C23 -179.4(5) . . . . ?
C26 C21 C22 C27 178.5(5) . . . . ?
B1 C21 C22 C27 -1.6(8) . . . . ?
C21 C22 C23 C24 0.8(9) . . . . ?
C27 C22 C23 C24 -177.1(6) . . . . ?
C22 C23 C24 C25 -1.0(9) . . . . ?
C22 C23 C24 C28 178.8(5) . . . . ?
C23 C24 C25 C26 -0.1(9) . . . . ?
C28 C24 C25 C26 -180.0(5) . . . . ?
C22 C21 C26 C25 -1.7(8) . . . . ?
B1 C21 C26 C25 178.4(5) . . . . ?
C22 C21 C26 C29 176.1(5) . . . . ?
B1 C21 C26 C29 -3.8(8) . . . . ?
C24 C25 C26 C21 1.5(9) . . . . ?
C24 C25 C26 C29 -176.4(6) . . . . ?

_refine_diff_density_max         0.528
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.085



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

data_9_wa3200_revised_by_AVirovets
_database_code_depnum_ccdc_archive 'CCDC 2384689'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_THETM01_9_wa3200_revised_by_AVirovets 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals scattered very weakly, showing almost no reflections 
above dhkl=1.0 A. Therefore, all the data above the diffraction limit
were discarded. 
;
_vrf_RINTA01_9_wa3200_revised_by_AVirovets 
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: The crystals scattered very weakly, so we even had to cut
the data above dhkl=1.0 A. 
;
_vrf_PLAT340_9_wa3200_revised_by_AVirovets 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.013 Ang.  
RESPONSE: The crystals scattered very weakly, so we even had to cut
the data above dhkl=1.0 A. 
;
_vrf_PLAT910_9_wa3200_revised_by_AVirovets 
;
RESPONSE: These reflections are hidden by the beamstop.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H16 O S4 [+ solvent]'
_chemical_formula_sum            'C21 H16 O S4'
_chemical_formula_weight         412.58

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   28.003(7)
_cell_length_b                   5.6280(12)
_cell_length_c                   28.991(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.94(2)
_cell_angle_gamma                90
_cell_volume                     4558.2(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1197
_cell_measurement_theta_min      4.1360
_cell_measurement_theta_max      25.8860

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.423
_shelx_estimated_absorpt_T_min   0.951
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_T_min  0.03164
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.034 0.000 413 161 'unknown solvent'
2 0.500 -0.003 0.500 413 161 'unknown solvent'
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            15410
_diffrn_reflns_av_unetI/netI     0.2862
_diffrn_reflns_av_R_equivalents  0.1950
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.646
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_full        20.815
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4758
_reflns_number_gt                2016
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_molecular_graphics    ?
_computing_publication_material  'IUCr PublCIF online service'

_refine_special_details          
'SQUEEZE,The crystals scattered very weakly, all data above dhkl=1.0 A were discarded'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4758
_refine_ls_number_parameters     471
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1609
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   0.690
_refine_ls_restrained_S_all      0.689
_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
S1 S 0.32880(11) 0.0815(5) 0.61446(9) 0.0404(8) Uani 1 1 d . . . . .
S2 S 0.22478(11) 0.8400(4) 0.51315(9) 0.0405(8) Uani 1 1 d . . . . .
S3 S 0.30522(9) 0.3337(4) 0.83479(8) 0.0236(6) Uani 1 1 d . . . . .
S4 S 0.40083(11) -0.4839(4) 0.92819(9) 0.0364(8) Uani 1 1 d . . . . .
O1 O 0.3649(3) -0.1487(11) 0.6920(2) 0.048(2) Uani 1 1 d . . . . .
C1 C 0.3376(4) 0.0358(16) 0.6737(3) 0.034(3) Uani 1 1 d . . . . .
C2 C 0.3139(3) 0.1929(15) 0.7005(3) 0.022(2) Uani 1 1 d . . . . .
C3 C 0.2889(3) 0.3633(14) 0.6703(3) 0.022(2) Uani 1 1 d . . . . .
H3 H 0.270980 0.491178 0.681710 0.026 Uiso 1 1 calc R U . . .
C4 C 0.2932(3) 0.3263(15) 0.6241(3) 0.025(3) Uani 1 1 d . . . . .
C5 C 0.2721(3) 0.4710(16) 0.5859(3) 0.027(3) Uani 1 1 d . . . . .
H5 H 0.254323 0.606955 0.593929 0.032 Uiso 1 1 calc R U . . .
C6 C 0.2754(4) 0.4299(17) 0.5403(3) 0.032(3) Uani 1 1 d . . . . .
H6 H 0.292640 0.292857 0.531960 0.038 Uiso 1 1 calc R U . . .
C7 C 0.2550(3) 0.5759(16) 0.5034(3) 0.028(3) Uani 1 1 d . . . . .
C8 C 0.2567(4) 0.5367(16) 0.4573(4) 0.035(3) Uani 1 1 d . . . . .
H8 H 0.271835 0.402466 0.444828 0.042 Uiso 1 1 calc R U . . .
C9 C 0.2334(4) 0.7161(17) 0.4296(4) 0.051(4) Uani 1 1 d . . . . .
H9 H 0.231012 0.714933 0.396723 0.062 Uiso 1 1 calc R U . . .
C10 C 0.2154(4) 0.8868(19) 0.4553(3) 0.042(3) Uani 1 1 d . . . . .
H10 H 0.198984 1.021586 0.442508 0.051 Uiso 1 1 calc R U . . .
C11 C 0.2960(3) 0.3759(15) 0.7766(3) 0.018(2) Uani 1 1 d . . . . .
H11 H 0.278978 0.507680 0.763233 0.021 Uiso 1 1 calc R U . . .
C12 C 0.3156(3) 0.2023(15) 0.7511(3) 0.021(2) Uani 1 1 d . . . . .
C13 C 0.3364(3) 0.0277(15) 0.7810(3) 0.019(2) Uani 1 1 d . . . . .
H13 H 0.350571 -0.111528 0.769419 0.023 Uiso 1 1 calc R U . . .
C14 C 0.3352(3) 0.0673(14) 0.8266(3) 0.015(2) Uani 1 1 d . U . . .
C15 C 0.3536(3) -0.0885(15) 0.8632(3) 0.022(2) Uani 1 1 d . . . . .
H15 H 0.368860 -0.229168 0.853598 0.026 Uiso 1 1 calc R U . . .
C16 C 0.3518(3) -0.0595(14) 0.9098(3) 0.018(2) Uani 1 1 d . . . . .
H16 H 0.335948 0.076782 0.920565 0.022 Uiso 1 1 calc R U . . .
C17 C 0.3725(3) -0.2230(14) 0.9434(3) 0.016(2) Uani 1 1 d . . . . .
C18 C 0.3761(4) -0.1935(16) 0.9909(3) 0.030(3) Uani 1 1 d . . . . .
H18 H 0.363014 -0.062701 1.006486 0.036 Uiso 1 1 calc R U . . .
C19 C 0.4022(4) -0.3864(17) 1.0139(3) 0.043(3) Uani 1 1 d . . . . .
H19 H 0.408385 -0.396210 1.046434 0.052 Uiso 1 1 calc R U . . .
C20 C 0.4170(4) -0.5514(17) 0.9840(4) 0.040(3) Uani 1 1 d . . . . .
H20 H 0.434442 -0.689963 0.993340 0.048 Uiso 1 1 calc R U . . .
C21 C 0.3943(4) -0.2727(17) 0.6608(4) 0.057(4) Uani 1 1 d . . . . .
H21A H 0.415727 -0.382253 0.678483 0.086 Uiso 1 1 calc R U . . .
H21B H 0.413283 -0.157569 0.644571 0.086 Uiso 1 1 calc R U . . .
H21C H 0.373764 -0.362565 0.638317 0.086 Uiso 1 1 calc R U . . .
S1A S 0.39766(9) 1.1445(4) 0.32187(9) 0.0349(7) Uani 1 1 d . . . . .
S2A S 0.48715(10) 0.3637(4) 0.22701(10) 0.0372(8) Uani 1 1 d . . . . .
S3A S 0.16864(9) 0.8572(4) 0.30684(9) 0.0272(7) Uani 1 1 d . . . . .
S4A S 0.07193(10) 1.6274(4) 0.40102(9) 0.0363(8) Uani 1 1 d . . . . .
O1A O 0.3229(2) 1.3720(11) 0.3575(2) 0.042(2) Uani 1 1 d . . . . .
C1A C 0.3378(3) 1.1870(16) 0.3330(3) 0.023(3) Uani 1 1 d . . . . .
C2A C 0.3074(4) 1.0247(15) 0.3110(3) 0.019(2) Uani 1 1 d . . . . .
C3A C 0.3349(3) 0.8603(15) 0.2865(3) 0.025(2) Uani 1 1 d . . . . .
H3A H 0.320371 0.732969 0.269282 0.030 Uiso 1 1 calc R U . . .
C4A C 0.3827(4) 0.8943(15) 0.2891(3) 0.029(3) Uani 1 1 d . . . . .
C5A C 0.4195(4) 0.7525(15) 0.2691(3) 0.034(3) Uani 1 1 d . . . . .
H5A H 0.408799 0.616672 0.251892 0.041 Uiso 1 1 calc R U . . .
C6A C 0.4671(4) 0.7920(16) 0.2721(3) 0.030(3) Uani 1 1 d . . . . .
H6A H 0.478762 0.927128 0.288963 0.036 Uiso 1 1 calc R U . . .
C7A C 0.5016(3) 0.6397(15) 0.2510(3) 0.026(3) Uani 1 1 d . . . . .
C8A C 0.5498(3) 0.6923(15) 0.2457(3) 0.025(3) Uani 1 1 d . . . . .
H8A H 0.565239 0.832898 0.257096 0.030 Uiso 1 1 calc R U . . .
C9A C 0.5728(3) 0.5131(15) 0.2216(3) 0.023(2) Uani 1 1 d . U . . .
H9A H 0.605488 0.520081 0.214944 0.028 Uiso 1 1 calc R U . . .
C10A C 0.5428(3) 0.3255(16) 0.2086(3) 0.031(3) Uani 1 1 d . . . . .
H10A H 0.552237 0.191777 0.191413 0.038 Uiso 1 1 calc R U . . .
C11A C 0.2278(4) 0.8294(16) 0.2955(3) 0.027(3) Uani 1 1 d . . . . .
H11A H 0.240208 0.702806 0.278215 0.032 Uiso 1 1 calc R U . . .
C12A C 0.2549(4) 1.0120(15) 0.3143(3) 0.021(2) Uani 1 1 d . . . . .
C13A C 0.2264(3) 1.1782(15) 0.3362(3) 0.025(3) Uani 1 1 d . . . . .
H13A H 0.239140 1.318617 0.350419 0.030 Uiso 1 1 calc R U . . .
C14A C 0.1789(3) 1.1215(14) 0.3353(3) 0.019(2) Uani 1 1 d . . . . .
C15A C 0.1422(4) 1.2675(15) 0.3557(3) 0.027(3) Uani 1 1 d . . . . .
H15A H 0.152540 1.407043 0.371938 0.032 Uiso 1 1 calc R U . . .
C16A C 0.0955(3) 1.2180(15) 0.3532(3) 0.024(3) Uani 1 1 d . U . . .
H16A H 0.085158 1.079673 0.336591 0.029 Uiso 1 1 calc R U . . .
C17A C 0.0597(3) 1.3572(15) 0.3736(3) 0.022(2) Uani 1 1 d . . . . .
C18A C 0.0124(3) 1.3095(15) 0.3749(3) 0.024(3) Uani 1 1 d . . . . .
H18A H -0.002139 1.173192 0.360660 0.028 Uiso 1 1 calc R U . . .
C19A C -0.0133(4) 1.4762(18) 0.3989(3) 0.039(3) Uani 1 1 d . . . . .
H19A H -0.046496 1.461480 0.403266 0.046 Uiso 1 1 calc R U . . .
C20A C 0.0145(4) 1.6654(18) 0.4155(3) 0.037(3) Uani 1 1 d . . . . .
H20A H 0.003203 1.796165 0.432445 0.044 Uiso 1 1 calc R U . . .
C21A C 0.3592(4) 1.5078(17) 0.3841(4) 0.050(3) Uani 1 1 d . . . . .
H21D H 0.344495 1.648610 0.397082 0.075 Uiso 1 1 calc R U . . .
H21E H 0.384075 1.557297 0.363957 0.075 Uiso 1 1 calc R U . . .
H21F H 0.373508 1.409189 0.409265 0.075 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C4 1.736(9) . ?
S1 C1 1.738(10) . ?
S2 C10 1.700(10) . ?
S2 C7 1.744(9) . ?
S3 C11 1.706(9) . ?
S3 C14 1.743(8) . ?
S4 C20 1.693(10) . ?
S4 C17 1.740(9) . ?
O1 C1 1.374(11) . ?
O1 C21 1.442(10) . ?
C1 C2 1.376(12) . ?
C2 C3 1.445(12) . ?
C2 C12 1.467(12) . ?
C3 C4 1.368(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.468(12) . ?
C5 C6 1.351(12) . ?
C5 H5 0.9500 . ?
C6 C7 1.436(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.358(12) . ?
C8 C9 1.420(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.337(13) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.361(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.409(11) . ?
C13 C14 1.342(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.444(12) . ?
C15 C16 1.366(11) . ?
C15 H15 0.9500 . ?
C16 C17 1.434(11) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(12) . ?
C18 C19 1.446(13) . ?
C18 H18 0.9500 . ?
C19 C20 1.353(12) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
S1A C4A 1.734(9) . ?
S1A C1A 1.746(9) . ?
S2A C10A 1.695(9) . ?
S2A C7A 1.739(9) . ?
S3A C14A 1.716(9) . ?
S3A C11A 1.719(10) . ?
S4A C20A 1.705(9) . ?
S4A C17A 1.739(9) . ?
O1A C1A 1.342(9) . ?
O1A C21A 1.450(11) . ?
C1A C2A 1.374(12) . ?
C2A C3A 1.423(11) . ?
C2A C12A 1.483(12) . ?
C3A C4A 1.347(12) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.457(12) . ?
C5A C6A 1.346(13) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.458(12) . ?
C6A H6A 0.9500 . ?
C7A C8A 1.399(12) . ?
C8A C9A 1.408(11) . ?
C8A H8A 0.9500 . ?
C9A C10A 1.385(12) . ?
C9A H9A 0.9500 . ?
C10A H10A 0.9500 . ?
C11A C12A 1.368(12) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.409(11) . ?
C13A C14A 1.365(12) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.472(12) . ?
C15A C16A 1.335(12) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.431(12) . ?
C16A H16A 0.9500 . ?
C17A C18A 1.355(12) . ?
C18A C19A 1.396(12) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.386(13) . ?
C19A H19A 0.9500 . ?
C20A H20A 0.9500 . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 S1 C1 90.1(5) . . ?
C10 S2 C7 90.9(5) . . ?
C11 S3 C14 91.5(4) . . ?
C20 S4 C17 92.5(5) . . ?
C1 O1 C21 116.8(7) . . ?
O1 C1 C2 123.0(9) . . ?
O1 C1 S1 122.0(7) . . ?
C2 C1 S1 115.0(8) . . ?
C1 C2 C3 108.5(8) . . ?
C1 C2 C12 127.2(9) . . ?
C3 C2 C12 124.2(8) . . ?
C4 C3 C2 114.8(8) . . ?
C4 C3 H3 122.6 . . ?
C2 C3 H3 122.6 . . ?
C3 C4 C5 126.7(8) . . ?
C3 C4 S1 111.6(7) . . ?
C5 C4 S1 121.6(7) . . ?
C6 C5 C4 126.4(9) . . ?
C6 C5 H5 116.8 . . ?
C4 C5 H5 116.8 . . ?
C5 C6 C7 125.5(9) . . ?
C5 C6 H6 117.3 . . ?
C7 C6 H6 117.3 . . ?
C8 C7 C6 127.0(9) . . ?
C8 C7 S2 110.4(7) . . ?
C6 C7 S2 122.6(8) . . ?
C7 C8 C9 113.3(9) . . ?
C7 C8 H8 123.3 . . ?
C9 C8 H8 123.3 . . ?
C10 C9 C8 111.8(11) . . ?
C10 C9 H9 124.1 . . ?
C8 C9 H9 124.1 . . ?
C9 C10 S2 113.7(9) . . ?
C9 C10 H10 123.2 . . ?
S2 C10 H10 123.2 . . ?
C12 C11 S3 113.4(7) . . ?
C12 C11 H11 123.3 . . ?
S3 C11 H11 123.3 . . ?
C11 C12 C13 109.4(8) . . ?
C11 C12 C2 125.6(8) . . ?
C13 C12 C2 124.9(8) . . ?
C14 C13 C12 116.8(8) . . ?
C14 C13 H13 121.6 . . ?
C12 C13 H13 121.6 . . ?
C13 C14 C15 126.2(8) . . ?
C13 C14 S3 108.8(7) . . ?
C15 C14 S3 124.9(7) . . ?
C16 C15 C14 128.3(8) . . ?
C16 C15 H15 115.9 . . ?
C14 C15 H15 115.9 . . ?
C15 C16 C17 123.8(8) . . ?
C15 C16 H16 118.1 . . ?
C17 C16 H16 118.1 . . ?
C18 C17 C16 126.7(8) . . ?
C18 C17 S4 110.6(7) . . ?
C16 C17 S4 122.6(7) . . ?
C17 C18 C19 111.6(8) . . ?
C17 C18 H18 124.2 . . ?
C19 C18 H18 124.2 . . ?
C20 C19 C18 112.8(9) . . ?
C20 C19 H19 123.6 . . ?
C18 C19 H19 123.6 . . ?
C19 C20 S4 112.6(8) . . ?
C19 C20 H20 123.7 . . ?
S4 C20 H20 123.7 . . ?
O1 C21 H21A 109.5 . . ?
O1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4A S1A C1A 90.7(5) . . ?
C10A S2A C7A 92.6(5) . . ?
C14A S3A C11A 92.2(5) . . ?
C20A S4A C17A 93.6(5) . . ?
C1A O1A C21A 117.4(8) . . ?
O1A C1A C2A 123.9(9) . . ?
O1A C1A S1A 122.7(7) . . ?
C2A C1A S1A 113.2(7) . . ?
C1A C2A C3A 109.0(9) . . ?
C1A C2A C12A 125.9(8) . . ?
C3A C2A C12A 125.0(8) . . ?
C4A C3A C2A 116.7(9) . . ?
C4A C3A H3A 121.7 . . ?
C2A C3A H3A 121.7 . . ?
C3A C4A C5A 128.9(9) . . ?
C3A C4A S1A 110.3(7) . . ?
C5A C4A S1A 120.8(8) . . ?
C6A C5A C4A 127.5(9) . . ?
C6A C5A H5A 116.3 . . ?
C4A C5A H5A 116.3 . . ?
C5A C6A C7A 123.9(9) . . ?
C5A C6A H6A 118.0 . . ?
C7A C6A H6A 118.0 . . ?
C8A C7A C6A 126.5(9) . . ?
C8A C7A S2A 110.2(6) . . ?
C6A C7A S2A 123.3(8) . . ?
C7A C8A C9A 112.3(8) . . ?
C7A C8A H8A 123.8 . . ?
C9A C8A H8A 123.8 . . ?
C10A C9A C8A 113.1(9) . . ?
C10A C9A H9A 123.5 . . ?
C8A C9A H9A 123.5 . . ?
C9A C10A S2A 111.8(7) . . ?
C9A C10A H10A 124.1 . . ?
S2A C10A H10A 124.1 . . ?
C12A C11A S3A 111.8(7) . . ?
C12A C11A H11A 124.1 . . ?
S3A C11A H11A 124.1 . . ?
C11A C12A C13A 111.2(9) . . ?
C11A C12A C2A 122.4(8) . . ?
C13A C12A C2A 126.4(8) . . ?
C14A C13A C12A 114.7(8) . . ?
C14A C13A H13A 122.7 . . ?
C12A C13A H13A 122.7 . . ?
C13A C14A C15A 124.6(8) . . ?
C13A C14A S3A 110.0(7) . . ?
C15A C14A S3A 125.4(7) . . ?
C16A C15A C14A 124.8(9) . . ?
C16A C15A H15A 117.6 . . ?
C14A C15A H15A 117.6 . . ?
C15A C16A C17A 125.1(9) . . ?
C15A C16A H16A 117.5 . . ?
C17A C16A H16A 117.5 . . ?
C18A C17A C16A 128.1(8) . . ?
C18A C17A S4A 108.8(7) . . ?
C16A C17A S4A 123.1(7) . . ?
C17A C18A C19A 114.8(9) . . ?
C17A C18A H18A 122.6 . . ?
C19A C18A H18A 122.6 . . ?
C20A C19A C18A 113.1(10) . . ?
C20A C19A H19A 123.4 . . ?
C18A C19A H19A 123.4 . . ?
C19A C20A S4A 109.5(7) . . ?
C19A C20A H20A 125.2 . . ?
S4A C20A H20A 125.2 . . ?
O1A C21A H21D 109.5 . . ?
O1A C21A H21E 109.5 . . ?
H21D C21A H21E 109.5 . . ?
O1A C21A H21F 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 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
C21 O1 C1 C2 -169.3(9) . . . . ?
C21 O1 C1 S1 12.9(13) . . . . ?
C4 S1 C1 O1 179.5(9) . . . . ?
C4 S1 C1 C2 1.5(8) . . . . ?
O1 C1 C2 C3 179.9(9) . . . . ?
S1 C1 C2 C3 -2.1(11) . . . . ?
O1 C1 C2 C12 3.8(16) . . . . ?
S1 C1 C2 C12 -178.2(7) . . . . ?
C1 C2 C3 C4 1.9(12) . . . . ?
C12 C2 C3 C4 178.1(8) . . . . ?
C2 C3 C4 C5 -179.5(9) . . . . ?
C2 C3 C4 S1 -0.8(10) . . . . ?
C1 S1 C4 C3 -0.4(7) . . . . ?
C1 S1 C4 C5 178.4(8) . . . . ?
C3 C4 C5 C6 -178.2(9) . . . . ?
S1 C4 C5 C6 3.1(14) . . . . ?
C4 C5 C6 C7 -179.0(9) . . . . ?
C5 C6 C7 C8 -178.2(10) . . . . ?
C5 C6 C7 S2 3.0(14) . . . . ?
C10 S2 C7 C8 0.1(8) . . . . ?
C10 S2 C7 C6 179.1(9) . . . . ?
C6 C7 C8 C9 -179.4(10) . . . . ?
S2 C7 C8 C9 -0.5(12) . . . . ?
C7 C8 C9 C10 0.7(14) . . . . ?
C8 C9 C10 S2 -0.6(13) . . . . ?
C7 S2 C10 C9 0.3(9) . . . . ?
C14 S3 C11 C12 -1.6(7) . . . . ?
S3 C11 C12 C13 2.7(10) . . . . ?
S3 C11 C12 C2 -179.2(7) . . . . ?
C1 C2 C12 C11 172.2(10) . . . . ?
C3 C2 C12 C11 -3.3(15) . . . . ?
C1 C2 C12 C13 -9.9(15) . . . . ?
C3 C2 C12 C13 174.6(9) . . . . ?
C11 C12 C13 C14 -2.8(12) . . . . ?
C2 C12 C13 C14 179.0(8) . . . . ?
C12 C13 C14 C15 178.9(8) . . . . ?
C12 C13 C14 S3 1.6(10) . . . . ?
C11 S3 C14 C13 0.0(7) . . . . ?
C11 S3 C14 C15 -177.3(8) . . . . ?
C13 C14 C15 C16 -177.6(9) . . . . ?
S3 C14 C15 C16 -0.8(14) . . . . ?
C14 C15 C16 C17 -178.1(8) . . . . ?
C15 C16 C17 C18 173.3(9) . . . . ?
C15 C16 C17 S4 -2.1(13) . . . . ?
C20 S4 C17 C18 0.0(8) . . . . ?
C20 S4 C17 C16 176.1(8) . . . . ?
C16 C17 C18 C19 -175.7(9) . . . . ?
S4 C17 C18 C19 0.1(11) . . . . ?
C17 C18 C19 C20 -0.3(13) . . . . ?
C18 C19 C20 S4 0.3(12) . . . . ?
C17 S4 C20 C19 -0.2(9) . . . . ?
C21A O1A C1A C2A 171.4(9) . . . . ?
C21A O1A C1A S1A -14.3(12) . . . . ?
C4A S1A C1A O1A -177.6(8) . . . . ?
C4A S1A C1A C2A -2.8(8) . . . . ?
O1A C1A C2A C3A 177.1(8) . . . . ?
S1A C1A C2A C3A 2.4(10) . . . . ?
O1A C1A C2A C12A -6.4(15) . . . . ?
S1A C1A C2A C12A 178.8(7) . . . . ?
C1A C2A C3A C4A -0.6(12) . . . . ?
C12A C2A C3A C4A -177.0(9) . . . . ?
C2A C3A C4A C5A 178.1(9) . . . . ?
C2A C3A C4A S1A -1.5(11) . . . . ?
C1A S1A C4A C3A 2.3(8) . . . . ?
C1A S1A C4A C5A -177.3(8) . . . . ?
C3A C4A C5A C6A 179.7(10) . . . . ?
S1A C4A C5A C6A -0.8(15) . . . . ?
C4A C5A C6A C7A 179.7(9) . . . . ?
C5A C6A C7A C8A 167.6(10) . . . . ?
C5A C6A C7A S2A -10.3(14) . . . . ?
C10A S2A C7A C8A -2.2(8) . . . . ?
C10A S2A C7A C6A 176.1(8) . . . . ?
C6A C7A C8A C9A -176.6(9) . . . . ?
S2A C7A C8A C9A 1.6(10) . . . . ?
C7A C8A C9A C10A 0.0(12) . . . . ?
C8A C9A C10A S2A -1.6(11) . . . . ?
C7A S2A C10A C9A 2.2(8) . . . . ?
C14A S3A C11A C12A 2.2(7) . . . . ?
S3A C11A C12A C13A -2.5(10) . . . . ?
S3A C11A C12A C2A 177.6(7) . . . . ?
C1A C2A C12A C11A -172.6(9) . . . . ?
C3A C2A C12A C11A 3.3(14) . . . . ?
C1A C2A C12A C13A 7.6(15) . . . . ?
C3A C2A C12A C13A -176.5(9) . . . . ?
C11A C12A C13A C14A 1.7(12) . . . . ?
C2A C12A C13A C14A -178.5(8) . . . . ?
C12A C13A C14A C15A -179.9(8) . . . . ?
C12A C13A C14A S3A 0.0(10) . . . . ?
C11A S3A C14A C13A -1.2(7) . . . . ?
C11A S3A C14A C15A 178.7(8) . . . . ?
C13A C14A C15A C16A 176.9(9) . . . . ?
S3A C14A C15A C16A -2.9(14) . . . . ?
C14A C15A C16A C17A 179.0(8) . . . . ?
C15A C16A C17A C18A -175.3(10) . . . . ?
C15A C16A C17A S4A 5.4(14) . . . . ?
C20A S4A C17A C18A 2.2(8) . . . . ?
C20A S4A C17A C16A -178.4(8) . . . . ?
C16A C17A C18A C19A 177.8(9) . . . . ?
S4A C17A C18A C19A -2.8(11) . . . . ?
C17A C18A C19A C20A 2.1(13) . . . . ?
C18A C19A C20A S4A -0.4(12) . . . . ?
C17A S4A C20A C19A -1.0(8) . . . . ?

_refine_diff_density_max         0.323
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.068



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

data_4_wa3339
_database_code_depnum_ccdc_archive 'CCDC 2384684'
loop_
_audit_author_name
_audit_author_address
'Alexander Virovets'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H6 Br2 S2'
_chemical_formula_sum            'C10 H6 Br2 S2'
_chemical_formula_weight         350.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   10.3682(4)
_cell_length_b                   7.5629(3)
_cell_length_c                   14.4299(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1131.49(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6554
_cell_measurement_theta_min      4.3950
_cell_measurement_theta_max      31.9850

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.055
_exptl_crystal_F_000             672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    7.488
_shelx_estimated_absorpt_T_min   0.246
_shelx_estimated_absorpt_T_max   0.662
_exptl_absorpt_correction_T_min  0.17094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_detector                 'image plate'
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_method       ω
_diffrn_reflns_number            21643
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.371
_diffrn_reflns_theta_max         29.120
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1516
_reflns_number_gt                1344
_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       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0234P)²+0.6857P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1516
_refine_ls_number_parameters     65
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0607
_refine_ls_wR_factor_gt          0.0591
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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
Br1 Br 0.38360(3) 0.51716(3) 0.90620(2) 0.04093(11) Uani 1 1 d . . . . .
S1 S 0.29885(5) 0.35615(7) 0.62169(4) 0.03085(14) Uani 1 1 d . . . . .
C1 C 0.27763(19) 0.3725(3) 0.73911(16) 0.0299(4) Uani 1 1 d . . . . .
H1 H 0.208070 0.320777 0.772305 0.036 Uiso 1 1 calc R U . . .
C2 C 0.37337(19) 0.4690(3) 0.77838(16) 0.0285(4) Uani 1 1 d . . . . .
C3 C 0.46529(19) 0.5349(3) 0.71397(16) 0.0291(4) Uani 1 1 d . . . . .
H3 H 0.537096 0.606254 0.730538 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4379(2) 0.4833(3) 0.62523(17) 0.0279(4) Uani 1 1 d . . . . .
C5 C 0.5124(2) 0.5273(3) 0.54313(17) 0.0311(5) Uani 1 1 d . . . . .
H5 H 0.585223 0.601801 0.551509 0.037 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C2 1.883(2) . ?
S1 C1 1.713(2) . ?
S1 C4 1.734(2) . ?
C1 C2 1.356(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.421(3) . ?
C3 C4 1.369(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.453(3) . ?
C5 C5 1.336(5) 5_666 ?
C5 H5 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 S1 C4 92.16(11) . . ?
C2 C1 S1 110.98(16) . . ?
C2 C1 H1 124.5 . . ?
S1 C1 H1 124.5 . . ?
C1 C2 C3 114.0(2) . . ?
C1 C2 Br1 123.68(17) . . ?
C3 C2 Br1 122.34(16) . . ?
C4 C3 C2 111.89(19) . . ?
C4 C3 H3 124.1 . . ?
C2 C3 H3 124.1 . . ?
C3 C4 C5 125.99(19) . . ?
C3 C4 S1 110.98(17) . . ?
C5 C4 S1 123.02(18) . . ?
C5 C5 C4 125.9(3) 5_666 . ?
C5 C5 H5 117.0 5_666 . ?
C4 C5 H5 117.0 . . ?

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
C4 S1 C1 C2 -0.59(16) . . . . ?
S1 C1 C2 C3 1.0(2) . . . . ?
S1 C1 C2 Br1 179.81(11) . . . . ?
C1 C2 C3 C4 -1.1(3) . . . . ?
Br1 C2 C3 C4 -179.85(14) . . . . ?
C2 C3 C4 C5 -179.89(19) . . . . ?
C2 C3 C4 S1 0.6(2) . . . . ?
C1 S1 C4 C3 0.00(17) . . . . ?
C1 S1 C4 C5 -179.56(18) . . . . ?
C3 C4 C5 C5 178.0(3) . . . 5_666 ?
S1 C4 C5 C5 -2.6(4) . . . 5_666 ?

_refine_diff_density_max         0.326
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.068


####################################################################### 
# 
# 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_5_wa3210
_database_code_depnum_ccdc_archive 'CCDC 2384685'
loop_
_audit_author_name
_audit_author_address
'Dr. Michael Bolte'
;Goethe University of Frankfurt
Germany
;
_audit_update_record             
;
2024-09-17 deposited with the CCDC.	2024-11-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H16 O2 S4'
_chemical_formula_sum            'C20 H16 O2 S4'
_chemical_formula_weight         416.57

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      orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   35.371(2)
_cell_length_b                   38.7786(17)
_cell_length_c                   5.5772(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7650.0(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    13908
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      26.17

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_F_000             3456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.509
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.335
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13908
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.356
_diffrn_reflns_theta_max         25.687
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3586
_reflns_number_gt                3016
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    0.999

_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       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0383P)²+58.5622P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1066 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.01(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3586
_refine_ls_number_parameters     235
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1379
_refine_ls_wR_factor_gt          0.1238
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_restrained_S_all      1.163
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.97938(6) 0.82878(7) 0.1933(8) 0.0886(12) Uani 1 1 d . . . . .
S2 S 0.81389(5) 0.76347(5) -0.0987(3) 0.0373(4) Uani 1 1 d . . . . .
S3 S 0.62179(6) 0.58241(6) 0.6297(5) 0.0542(6) Uani 1 1 d . . . . .
S4 S 0.77146(4) 0.67520(5) 0.7047(3) 0.0340(4) Uani 1 1 d . . . . .
O1 O 0.94491(18) 0.77187(17) 0.3677(17) 0.090(3) Uani 1 1 d . . . . .
O2 O 0.68723(15) 0.59026(14) 0.8789(12) 0.0549(15) Uani 1 1 d . . . . .
C1 C 0.9429(2) 0.7991(2) 0.216(2) 0.060(3) Uani 1 1 d . . . . .
C2 C 0.9137(2) 0.80582(18) 0.0654(16) 0.045(2) Uani 1 1 d . . . . .
C3 C 0.9211(3) 0.8359(2) -0.071(2) 0.061(3) Uani 1 1 d . . . . .
H3 H 0.904202 0.844837 -0.188000 0.074 Uiso 1 1 calc R U . . .
C4 C 0.9552(3) 0.8506(3) -0.018(3) 0.090(4) Uani 1 1 d . . . . .
H4 H 0.964324 0.871082 -0.092079 0.108 Uiso 1 1 calc R U . . .
C5 C 0.9710(3) 0.7720(3) 0.559(2) 0.086(4) Uani 1 1 d . . . . .
H5A H 0.968650 0.750483 0.650083 0.130 Uiso 1 1 calc R U . . .
H5B H 0.996738 0.773941 0.495167 0.130 Uiso 1 1 calc R U . . .
H5C H 0.965786 0.791616 0.664566 0.130 Uiso 1 1 calc R U . . .
C6 C 0.8533(2) 0.78870(18) -0.1340(15) 0.0418(18) Uani 1 1 d . . . . .
H6 H 0.857252 0.803221 -0.268867 0.050 Uiso 1 1 calc R U . . .
C7 C 0.87828(18) 0.78591(16) 0.0496(14) 0.0347(16) Uani 1 1 d . . . . .
C8 C 0.86470(17) 0.76273(16) 0.2250(13) 0.0302(14) Uani 1 1 d . . . . .
H8 H 0.878362 0.757528 0.367122 0.036 Uiso 1 1 calc R U . . .
C9 C 0.83029(16) 0.74837(16) 0.1739(12) 0.0285(14) Uani 1 1 d . . . . .
C10 C 0.80950(18) 0.72437(16) 0.3183(13) 0.0312(15) Uani 1 1 d . . . . .
H10 H 0.821867 0.716290 0.458666 0.037 Uiso 1 1 calc R U . . .
C11 C 0.66517(19) 0.60107(18) 0.6982(15) 0.0403(18) Uani 1 1 d . . . . .
C12 C 0.67369(17) 0.62800(17) 0.5511(14) 0.0338(16) Uani 1 1 d . . . . .
C13 C 0.64474(19) 0.63344(18) 0.3780(15) 0.0434(19) Uani 1 1 d . . . . .
H13 H 0.645927 0.650927 0.258927 0.052 Uiso 1 1 calc R U . . .
C14 C 0.6152(2) 0.6112(2) 0.3994(18) 0.056(2) Uani 1 1 d . . . . .
H14 H 0.593510 0.611495 0.298960 0.067 Uiso 1 1 calc R U . . .
C15 C 0.6765(3) 0.5596(2) 0.999(2) 0.068(3) Uani 1 1 d . . . . .
H15A H 0.694770 0.554560 1.126138 0.102 Uiso 1 1 calc R U . . .
H15B H 0.651316 0.562642 1.069343 0.102 Uiso 1 1 calc R U . . .
H15C H 0.675923 0.540471 0.884370 0.102 Uiso 1 1 calc R U . . .
C16 C 0.73368(18) 0.64817(17) 0.7509(14) 0.0344(16) Uani 1 1 d . . . . .
H16 H 0.730580 0.634389 0.890325 0.041 Uiso 1 1 calc R U . . .
C17 C 0.70861(16) 0.64872(15) 0.5648(13) 0.0291(15) Uani 1 1 d . . . . .
C18 C 0.72029(16) 0.67225(15) 0.3821(14) 0.0289(14) Uani 1 1 d . . . . .
H18 H 0.705974 0.676486 0.241066 0.035 Uiso 1 1 calc R U . . .
C19 C 0.75418(16) 0.68820(15) 0.4295(13) 0.0277(14) Uani 1 1 d . . . . .
C20 C 0.77450(17) 0.71191(17) 0.2784(13) 0.0316(15) Uani 1 1 d . . . . .
H20 H 0.762039 0.719496 0.136997 0.038 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C4 1.684(15) . ?
S1 C1 1.733(8) . ?
S2 C6 1.714(7) . ?
S2 C9 1.730(7) . ?
S3 C14 1.717(9) . ?
S3 C11 1.739(7) . ?
S4 C16 1.717(7) . ?
S4 C19 1.727(7) . ?
O1 C1 1.355(13) . ?
O1 C5 1.411(13) . ?
O2 C11 1.342(9) . ?
O2 C15 1.416(9) . ?
C1 C2 1.359(13) . ?
C2 C3 1.418(11) . ?
C2 C7 1.473(9) . ?
C3 C4 1.368(13) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.357(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.413(10) . ?
C8 C9 1.368(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.434(9) . ?
C10 C20 1.348(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.362(10) . ?
C12 C13 1.423(10) . ?
C12 C17 1.475(8) . ?
C13 C14 1.361(10) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.365(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.429(9) . ?
C18 C19 1.374(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.440(9) . ?
C20 H20 0.9500 . ?

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
C4 S1 C1 90.5(5) . . ?
C6 S2 C9 91.2(4) . . ?
C14 S3 C11 90.8(4) . . ?
C16 S4 C19 92.1(3) . . ?
C1 O1 C5 120.2(8) . . ?
C11 O2 C15 117.5(6) . . ?
O1 C1 C2 125.1(7) . . ?
O1 C1 S1 121.7(7) . . ?
C2 C1 S1 113.2(8) . . ?
C1 C2 C3 110.4(8) . . ?
C1 C2 C7 125.7(7) . . ?
C3 C2 C7 123.8(8) . . ?
C4 C3 C2 113.0(10) . . ?
C4 C3 H3 123.5 . . ?
C2 C3 H3 123.5 . . ?
C3 C4 S1 112.9(8) . . ?
C3 C4 H4 123.6 . . ?
S1 C4 H4 123.6 . . ?
O1 C5 H5A 109.5 . . ?
O1 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O1 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 S2 113.4(6) . . ?
C7 C6 H6 123.3 . . ?
S2 C6 H6 123.3 . . ?
C6 C7 C8 110.6(6) . . ?
C6 C7 C2 123.8(7) . . ?
C8 C7 C2 125.5(7) . . ?
C9 C8 C7 114.7(7) . . ?
C9 C8 H8 122.7 . . ?
C7 C8 H8 122.7 . . ?
C8 C9 C10 127.1(7) . . ?
C8 C9 S2 110.1(5) . . ?
C10 C9 S2 122.8(5) . . ?
C20 C10 C9 127.7(6) . . ?
C20 C10 H10 116.2 . . ?
C9 C10 H10 116.2 . . ?
O2 C11 C12 124.3(6) . . ?
O2 C11 S3 123.2(5) . . ?
C12 C11 S3 112.5(5) . . ?
C11 C12 C13 111.3(6) . . ?
C11 C12 C17 124.9(6) . . ?
C13 C12 C17 123.8(6) . . ?
C14 C13 C12 113.5(7) . . ?
C14 C13 H13 123.2 . . ?
C12 C13 H13 123.2 . . ?
C13 C14 S3 111.9(6) . . ?
C13 C14 H14 124.0 . . ?
S3 C14 H14 124.0 . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 S4 112.4(5) . . ?
C17 C16 H16 123.8 . . ?
S4 C16 H16 123.8 . . ?
C16 C17 C18 111.4(6) . . ?
C16 C17 C12 125.1(6) . . ?
C18 C17 C12 123.6(6) . . ?
C19 C18 C17 113.7(6) . . ?
C19 C18 H18 123.1 . . ?
C17 C18 H18 123.1 . . ?
C18 C19 C20 127.6(6) . . ?
C18 C19 S4 110.4(5) . . ?
C20 C19 S4 122.0(5) . . ?
C10 C20 C19 126.2(6) . . ?
C10 C20 H20 116.9 . . ?
C19 C20 H20 116.9 . . ?

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
C5 O1 C1 C2 -163.0(9) . . . . ?
C5 O1 C1 S1 18.3(13) . . . . ?
C4 S1 C1 O1 179.2(9) . . . . ?
C4 S1 C1 C2 0.4(7) . . . . ?
O1 C1 C2 C3 -178.8(9) . . . . ?
S1 C1 C2 C3 0.0(9) . . . . ?
O1 C1 C2 C7 3.4(14) . . . . ?
S1 C1 C2 C7 -177.8(6) . . . . ?
C1 C2 C3 C4 -0.5(11) . . . . ?
C7 C2 C3 C4 177.4(8) . . . . ?
C2 C3 C4 S1 0.8(11) . . . . ?
C1 S1 C4 C3 -0.7(8) . . . . ?
C9 S2 C6 C7 0.6(6) . . . . ?
S2 C6 C7 C8 -0.5(8) . . . . ?
S2 C6 C7 C2 -177.9(5) . . . . ?
C1 C2 C7 C6 -165.6(8) . . . . ?
C3 C2 C7 C6 16.9(11) . . . . ?
C1 C2 C7 C8 17.5(11) . . . . ?
C3 C2 C7 C8 -160.0(7) . . . . ?
C6 C7 C8 C9 0.1(8) . . . . ?
C2 C7 C8 C9 177.4(6) . . . . ?
C7 C8 C9 C10 -179.5(6) . . . . ?
C7 C8 C9 S2 0.3(7) . . . . ?
C6 S2 C9 C8 -0.5(5) . . . . ?
C6 S2 C9 C10 179.3(6) . . . . ?
C8 C9 C10 C20 174.9(6) . . . . ?
S2 C9 C10 C20 -4.8(9) . . . . ?
C15 O2 C11 C12 -173.3(8) . . . . ?
C15 O2 C11 S3 7.9(11) . . . . ?
C14 S3 C11 O2 179.2(7) . . . . ?
C14 S3 C11 C12 0.2(7) . . . . ?
O2 C11 C12 C13 -179.6(8) . . . . ?
S3 C11 C12 C13 -0.6(9) . . . . ?
O2 C11 C12 C17 1.4(12) . . . . ?
S3 C11 C12 C17 -179.6(6) . . . . ?
C11 C12 C13 C14 0.8(10) . . . . ?
C17 C12 C13 C14 179.9(7) . . . . ?
C12 C13 C14 S3 -0.6(10) . . . . ?
C11 S3 C14 C13 0.3(8) . . . . ?
C19 S4 C16 C17 0.1(6) . . . . ?
S4 C16 C17 C18 -1.0(7) . . . . ?
S4 C16 C17 C12 179.2(5) . . . . ?
C11 C12 C17 C16 -12.9(11) . . . . ?
C13 C12 C17 C16 168.2(7) . . . . ?
C11 C12 C17 C18 167.4(7) . . . . ?
C13 C12 C17 C18 -11.5(11) . . . . ?
C16 C17 C18 C19 1.7(8) . . . . ?
C12 C17 C18 C19 -178.5(6) . . . . ?
C17 C18 C19 C20 176.9(6) . . . . ?
C17 C18 C19 S4 -1.6(7) . . . . ?
C16 S4 C19 C18 0.9(5) . . . . ?
C16 S4 C19 C20 -177.8(6) . . . . ?
C9 C10 C20 C19 -178.9(6) . . . . ?
C18 C19 C20 C10 -172.6(6) . . . . ?
S4 C19 C20 C10 5.8(9) . . . . ?

_refine_diff_density_max         0.239
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.063


