#------------------------------------------------------------------------------
#$Date: 2025-05-14 13:17:04 +0300 (Wed, 14 May 2025) $
#$Revision: 299663 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/92/1569250.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1569250
loop_
_publ_author_name
'Qin, Wenjie'
'Ni, Qian'
'Jiao, Wenjun'
'Ma, Yuanhong'
_publ_section_title
;
 B(C₆F₅)₃-catalyzed regio- and
 stereoselective thiosulfonylation of terminal alkynes with
 thiosulfonates.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7951
_journal_page_last               7954
_journal_paper_doi               10.1039/d3cc02151c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C23 H22 O3 S2, 0.5(C H Cl3)'
_chemical_formula_sum            'C23.5 H22.5 Cl1.5 O3 S2'
_chemical_formula_weight         470.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2fhk9t
_audit_creation_date             2023-01-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-16 deposited with the CCDC.	2023-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                113.174(4)
_cell_angle_beta                 97.818(3)
_cell_angle_gamma                97.371(3)
_cell_formula_units_Z            4
_cell_length_a                   9.9799(3)
_cell_length_b                   15.1960(6)
_cell_length_c                   16.9612(7)
_cell_measurement_reflns_used    5213
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.2460
_cell_measurement_theta_min      2.9270
_cell_volume                     2295.56(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0697
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     58.00 102.00   1.00    1.00    --   34.48  57.00 -30.00   44
  2  ω     36.00 112.00   1.00    6.00    --  105.25 -30.00 -30.00   76
  3  ω     69.00 125.00   1.00    6.00    --  105.25 -30.00-120.00   56
  4  ω     85.00 127.00   1.00    6.00    --  105.25 -30.00-180.00   42
  5  ω     84.00 116.00   1.00    6.00    --  105.25-111.00 -90.00   32
  6  ω     46.00  83.00   1.00    1.00    --   34.48-125.00 -30.00   37
  7  ω    104.00 130.00   1.00    6.00    --  105.25 111.00-120.00   26
  8  ω     35.00  69.00   1.00    6.00    --  105.25 -30.00-180.00   34
  9  ω     38.00 115.00   1.00    6.00    --  105.25 -61.00-120.00   77
 10  ω     36.00  98.00   1.00    6.00    --  105.25 -94.00-150.00   62
 11  ω     39.00  65.00   1.00    6.00    --  105.25-111.00 -90.00   26
 12  ω     48.00 115.00   1.00    6.00    --  105.25-111.00  30.00   67
 13  ω     83.00 108.00   1.00    6.00    --  105.25 -94.00 120.00   25
 14  ω     37.00  86.00   1.00    1.00    --   34.48-125.00 120.00   49
 15  ω     38.00 118.00   1.00    6.00    --  105.25 -45.00  60.00   80
 16  ω     99.00 165.00   1.00    6.00    --  105.25  30.00 150.00   66
 17  ω     38.00 140.00   1.00    6.00    --  105.25 -15.00 120.00  102
 18  ω     39.00 135.00   1.00    6.00    --  105.25 -82.00  46.00   96
 19  ω     24.00  63.00   1.00    1.00    --   34.48 -19.00 150.00   39
 20  ω     23.00  89.00   1.00    1.00    --   34.48  38.00  60.00   66
 21  ω     23.00  84.00   1.00    1.00    --   34.48  38.00 -30.00   61
 22  ω      9.00  87.00   1.00    1.00    --   34.48  77.00-150.00   78
 23  ω    -29.00  51.00   1.00    1.00    --   34.48 -57.00  90.00   80
 24  ω    -37.00  -4.00   1.00    1.00    --   34.48 -19.00 150.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0489024000
_diffrn_orient_matrix_UB_12      -0.0841494000
_diffrn_orient_matrix_UB_13      0.0249189000
_diffrn_orient_matrix_UB_21      0.0375055000
_diffrn_orient_matrix_UB_22      -0.0732042000
_diffrn_orient_matrix_UB_23      -0.0828926000
_diffrn_orient_matrix_UB_31      0.1465880000
_diffrn_orient_matrix_UB_32      0.0150309000
_diffrn_orient_matrix_UB_33      0.0519213000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14124
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        66.574
_diffrn_reflns_theta_max         66.574
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       needle
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0689P)²+2.0619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1733
_refine_ls_wR_factor_ref         0.1859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5605
_reflns_number_total             7991
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc02151c2.cif
_cod_data_source_block           exp_2752
_cod_depositor_comments
;
          Adding full bibliography for 1569250.cif.

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C47 H45 Cl3 O6 S4'
_cod_original_formula_weight         940.42
_cod_original_formula_moiety         '2(C23 H22 O3 S2), C H Cl3'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2295.56(16)
_cod_database_code               1569250
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C100 H100 S1 O6'
_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.
;
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C47(H47)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C29(H29), C30(H30), C33(H33), C34(H34), C36(H36),
 C37(H37), C38(H38), C41(H41), C42(H42), C44(H44), C45(H45), C3(H3), C4(H4),
 C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C15(H15), C17(H17),
 C19(H19), C20(H20), C22(H22)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C46(H46A,H46B,H46C), C1(H1A,H1B,
 H1C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.663
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.75767(12) 0.05994(7) 0.54706(6) 0.0547(3) Uani 1 1 d . . . . .
O1 O 0.9958(4) 0.0372(3) 0.8307(2) 0.0774(10) Uani 1 1 d . . . . .
S2 S 0.93119(12) 0.11187(8) 0.81866(7) 0.0578(3) Uani 1 1 d . . . . .
O2 O 1.0121(3) 0.2081(2) 0.8488(2) 0.0705(9) Uani 1 1 d . . . . .
O6 O 0.7926(4) 0.5104(2) 0.7885(2) 0.0746(9) Uani 1 1 d . . . . .
C24 C 0.4272(7) 0.1380(6) 0.9815(5) 0.108(2) Uani 1 1 d . . . . .
H24A H 0.440111 0.200389 1.030293 0.162 Uiso 1 1 calc GR . . . .
H24B H 0.412124 0.087076 1.001302 0.162 Uiso 1 1 calc GR . . . .
H24C H 0.348539 0.130465 0.938278 0.162 Uiso 1 1 calc GR . . . .
C25 C 0.5547(6) 0.1318(4) 0.9417(3) 0.0752(14) Uani 1 1 d . . . . .
C26 C 0.5901(6) 0.0425(4) 0.8976(4) 0.0808(15) Uani 1 1 d . . . . .
H26 H 0.534731 -0.014380 0.892457 0.097 Uiso 1 1 calc R . . . .
C27 C 0.7049(6) 0.0366(3) 0.8616(3) 0.0734(13) Uani 1 1 d . . . . .
H27 H 0.727702 -0.023844 0.832952 0.088 Uiso 1 1 calc R . . . .
C28 C 0.7870(5) 0.1202(3) 0.8675(3) 0.0560(10) Uani 1 1 d . . . . .
C29 C 0.7544(5) 0.2101(3) 0.9116(3) 0.0685(12) Uani 1 1 d . . . . .
H29 H 0.809521 0.266932 0.916353 0.082 Uiso 1 1 calc R . . . .
C30 C 0.6386(6) 0.2146(4) 0.9485(4) 0.0784(14) Uani 1 1 d . . . . .
H30 H 0.617027 0.275148 0.978700 0.094 Uiso 1 1 calc R . . . .
C31 C 0.6644(6) 0.5405(4) 0.7964(4) 0.0885(17) Uani 1 1 d . . . . .
H31A H 0.600164 0.506297 0.741394 0.133 Uiso 1 1 calc GR . . . .
H31B H 0.677496 0.609498 0.812526 0.133 Uiso 1 1 calc GR . . . .
H31C H 0.628679 0.525982 0.840679 0.133 Uiso 1 1 calc GR . . . .
C32 C 0.7929(5) 0.4132(3) 0.7600(3) 0.0543(10) Uani 1 1 d . . . . .
C33 C 0.6804(5) 0.3426(3) 0.7464(3) 0.0626(11) Uani 1 1 d . . . . .
H33 H 0.596768 0.359882 0.758056 0.075 Uiso 1 1 calc R . . . .
C34 C 0.6928(4) 0.2450(3) 0.7150(3) 0.0603(11) Uani 1 1 d . . . . .
H34 H 0.616545 0.197243 0.705379 0.072 Uiso 1 1 calc R . . . .
C35 C 0.8153(4) 0.2183(3) 0.6981(2) 0.0445(8) Uani 1 1 d . . . . .
C36 C 0.9279(4) 0.2896(3) 0.7119(3) 0.0563(10) Uani 1 1 d . . . . .
H36 H 1.011608 0.272364 0.700466 0.068 Uiso 1 1 calc R . . . .
C37 C 0.9164(4) 0.3862(3) 0.7425(3) 0.0609(11) Uani 1 1 d . . . . .
H37 H 0.992605 0.433791 0.751574 0.073 Uiso 1 1 calc R . . . .
C38 C 0.8654(5) 0.0632(3) 0.7058(3) 0.0540(10) Uani 1 1 d . . . . .
H38 H 0.860314 -0.003321 0.674225 0.065 Uiso 1 1 calc R . . . .
C39 C 0.8220(4) 0.1123(3) 0.6608(2) 0.0470(8) Uani 1 1 d . . . . .
C40 C 0.7607(4) -0.0669(3) 0.5108(2) 0.0481(9) Uani 1 1 d . . . . .
C41 C 0.8837(4) -0.1004(3) 0.5106(3) 0.0546(10) Uani 1 1 d . . . . .
H41 H 0.967544 -0.056115 0.533658 0.065 Uiso 1 1 calc R . . . .
C42 C 0.8814(5) -0.1989(3) 0.4762(3) 0.0578(10) Uani 1 1 d . . . . .
H42 H 0.964419 -0.220587 0.476568 0.069 Uiso 1 1 calc R . . . .
C43 C 0.7578(5) -0.2673(3) 0.4407(3) 0.0581(11) Uani 1 1 d . . . . .
C44 C 0.6381(5) -0.2323(3) 0.4417(3) 0.0616(11) Uani 1 1 d . . . . .
H44 H 0.554450 -0.276774 0.418382 0.074 Uiso 1 1 calc R . . . .
C45 C 0.6364(4) -0.1332(3) 0.4760(3) 0.0587(10) Uani 1 1 d . . . . .
H45 H 0.553219 -0.111708 0.475622 0.070 Uiso 1 1 calc R . . . .
C46 C 0.7583(6) -0.3753(3) 0.4025(3) 0.0801(15) Uani 1 1 d . . . . .
H46A H 0.822589 -0.388967 0.364069 0.120 Uiso 1 1 calc GR . . . .
H46B H 0.667537 -0.411262 0.370238 0.120 Uiso 1 1 calc GR . . . .
H46C H 0.785149 -0.394441 0.449062 0.120 Uiso 1 1 calc GR . . . .
C1 C 0.2035(5) -0.7773(3) 0.3183(3) 0.0693(12) Uani 1 1 d . . . . .
H1A H 0.273575 -0.789790 0.284058 0.104 Uiso 1 1 calc GR . . . .
H1B H 0.114496 -0.809907 0.281042 0.104 Uiso 1 1 calc GR . . . .
H1C H 0.219342 -0.801305 0.362681 0.104 Uiso 1 1 calc GR . . . .
C2 C 0.2081(4) -0.6689(3) 0.3611(3) 0.0517(9) Uani 1 1 d . . . . .
S3 S 0.22719(13) -0.33964(8) 0.47820(7) 0.0620(3) Uani 1 1 d . . . . .
O3 O 0.4821(3) -0.2203(2) 0.7750(2) 0.0696(9) Uani 1 1 d . . . . .
C3 C 0.0913(4) -0.6316(3) 0.3712(3) 0.0626(11) Uani 1 1 d . . . . .
H3 H 0.006247 -0.674379 0.351728 0.075 Uiso 1 1 calc R . . . .
S4 S 0.37181(11) -0.30184(7) 0.74991(6) 0.0520(3) Uani 1 1 d . . . . .
O4 O 0.3984(4) -0.3870(2) 0.7615(2) 0.0712(9) Uani 1 1 d . . . . .
C4 C 0.0954(4) -0.5316(3) 0.4098(3) 0.0611(11) Uani 1 1 d . . . . .
H4 H 0.013980 -0.508188 0.415671 0.073 Uiso 1 1 calc R . . . .
O5 O 0.3909(4) 0.1173(2) 0.7191(2) 0.0727(9) Uani 1 1 d . . . . .
C5 C 0.3398(5) -0.5040(3) 0.4292(3) 0.0645(12) Uani 1 1 d . . . . .
H5 H 0.424953 -0.461376 0.448162 0.077 Uiso 1 1 calc R . . . .
C6 C 0.2207(4) -0.4674(3) 0.4392(2) 0.0520(9) Uani 1 1 d . . . . .
C7 C 0.3333(5) -0.6038(3) 0.3912(3) 0.0655(12) Uani 1 1 d . . . . .
H7 H 0.414532 -0.627575 0.385761 0.079 Uiso 1 1 calc R . . . .
C8 C 0.3011(4) -0.3460(3) 0.6375(3) 0.0512(9) Uani 1 1 d . . . . .
H8 H 0.272203 -0.413284 0.606587 0.061 Uiso 1 1 calc R . . . .
C9 C 0.2848(4) -0.2919(3) 0.5922(2) 0.0450(8) Uani 1 1 d . . . . .
C10 C 0.3107(4) -0.1833(3) 0.6290(2) 0.0446(8) Uani 1 1 d . . . . .
C11 C 0.4370(4) -0.1312(3) 0.6331(3) 0.0638(12) Uani 1 1 d . . . . .
H11 H 0.507296 -0.164213 0.615099 0.077 Uiso 1 1 calc R . . . .
C12 C 0.2079(4) -0.1331(3) 0.6539(3) 0.0560(10) Uani 1 1 d . . . . .
H12 H 0.121042 -0.167692 0.649235 0.067 Uiso 1 1 calc R . . . .
C13 C 0.2301(5) -0.0324(3) 0.6859(3) 0.0584(11) Uani 1 1 d . . . . .
H13 H 0.159835 0.000495 0.704333 0.070 Uiso 1 1 calc R . . . .
C14 C 0.3570(4) 0.0185(3) 0.6903(3) 0.0526(9) Uani 1 1 d . . . . .
C15 C 0.4606(5) -0.0320(3) 0.6632(4) 0.0687(13) Uani 1 1 d . . . . .
H15 H 0.546600 0.001961 0.665679 0.082 Uiso 1 1 calc R . . . .
C16 C 0.2859(7) 0.1712(4) 0.7418(4) 0.0902(18) Uani 1 1 d . . . . .
H16A H 0.209904 0.147470 0.692686 0.135 Uiso 1 1 calc GR . . . .
H16B H 0.321631 0.239042 0.757869 0.135 Uiso 1 1 calc GR . . . .
H16C H 0.254915 0.163810 0.790448 0.135 Uiso 1 1 calc GR . . . .
C17 C 0.2297(5) -0.1641(3) 0.8375(3) 0.0609(11) Uani 1 1 d . . . . .
H17 H 0.293102 -0.119118 0.829927 0.073 Uiso 1 1 calc R . . . .
C18 C 0.2407(4) -0.2615(3) 0.8064(2) 0.0491(9) Uani 1 1 d . . . . .
C19 C 0.1475(5) -0.3268(3) 0.8194(3) 0.0651(12) Uani 1 1 d . . . . .
H19 H 0.154549 -0.392187 0.799150 0.078 Uiso 1 1 calc R . . . .
C20 C 0.0435(6) -0.2951(4) 0.8625(3) 0.0778(14) Uani 1 1 d . . . . .
H20 H -0.018201 -0.339502 0.871888 0.093 Uiso 1 1 calc R . . . .
C21 C 0.0289(5) -0.1993(4) 0.8918(3) 0.0722(13) Uani 1 1 d . . . . .
C22 C 0.1247(6) -0.1344(4) 0.8795(3) 0.0712(13) Uani 1 1 d . . . . .
H22 H 0.117968 -0.069015 0.900262 0.085 Uiso 1 1 calc R . . . .
C23 C -0.0896(7) -0.1663(6) 0.9357(4) 0.111(2) Uani 1 1 d . . . . .
H23A H -0.061868 -0.098868 0.976509 0.167 Uiso 1 1 calc GR . . . .
H23B H -0.114194 -0.205288 0.966377 0.167 Uiso 1 1 calc GR . . . .
H23C H -0.167707 -0.173774 0.892133 0.167 Uiso 1 1 calc GR . . . .
Cl1 Cl 1.1736(4) 0.4984(2) 0.9944(2) 0.1866(13) Uani 1 1 d . . . . .
Cl2 Cl 1.2990(2) 0.46076(16) 0.84778(14) 0.1149(6) Uani 1 1 d . . . . .
Cl3 Cl 1.3644(3) 0.37210(16) 0.96380(15) 0.1472(9) Uani 1 1 d . . . . .
C47 C 1.2366(6) 0.4128(4) 0.9162(4) 0.0855(16) Uani 1 1 d . . . . .
H47 H 1.160874 0.357106 0.880871 0.103 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C39 S1 C40 105.57(18) . . ?
O1 S2 C28 108.3(2) . . ?
O1 S2 C38 104.2(2) . . ?
O2 S2 O1 118.8(2) . . ?
O2 S2 C28 108.4(2) . . ?
O2 S2 C38 110.7(2) . . ?
C28 S2 C38 105.7(2) . . ?
C32 O6 C31 118.0(4) . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
C26 C25 C24 120.9(6) . . ?
C30 C25 C24 120.9(6) . . ?
C30 C25 C26 118.2(5) . . ?
C25 C26 H26 119.4 . . ?
C27 C26 C25 121.1(5) . . ?
C27 C26 H26 119.4 . . ?
C26 C27 H27 119.9 . . ?
C26 C27 C28 120.2(5) . . ?
C28 C27 H27 119.9 . . ?
C27 C28 S2 120.0(4) . . ?
C27 C28 C29 119.8(5) . . ?
C29 C28 S2 120.2(4) . . ?
C28 C29 H29 120.4 . . ?
C28 C29 C30 119.1(5) . . ?
C30 C29 H29 120.4 . . ?
C25 C30 C29 121.6(5) . . ?
C25 C30 H30 119.2 . . ?
C29 C30 H30 119.2 . . ?
O6 C31 H31A 109.5 . . ?
O6 C31 H31B 109.5 . . ?
O6 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O6 C32 C33 124.8(4) . . ?
O6 C32 C37 115.8(4) . . ?
C33 C32 C37 119.5(4) . . ?
C32 C33 H33 120.3 . . ?
C32 C33 C34 119.4(4) . . ?
C34 C33 H33 120.3 . . ?
C33 C34 H34 119.4 . . ?
C35 C34 C33 121.2(4) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 C36 119.1(4) . . ?
C34 C35 C39 119.3(3) . . ?
C36 C35 C39 121.6(4) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 C35 120.1(4) . . ?
C37 C36 H36 119.9 . . ?
C32 C37 H37 119.6 . . ?
C36 C37 C32 120.7(4) . . ?
C36 C37 H37 119.6 . . ?
S2 C38 H38 116.9 . . ?
C39 C38 S2 126.2(3) . . ?
C39 C38 H38 116.9 . . ?
C35 C39 S1 109.4(3) . . ?
C38 C39 S1 124.4(3) . . ?
C38 C39 C35 126.1(4) . . ?
C41 C40 S1 121.8(3) . . ?
C45 C40 S1 118.3(3) . . ?
C45 C40 C41 119.8(4) . . ?
C40 C41 H41 120.1 . . ?
C42 C41 C40 119.9(4) . . ?
C42 C41 H41 120.1 . . ?
C41 C42 H42 119.2 . . ?
C41 C42 C43 121.6(4) . . ?
C43 C42 H42 119.2 . . ?
C42 C43 C46 120.5(4) . . ?
C44 C43 C42 117.3(4) . . ?
C44 C43 C46 122.2(4) . . ?
C43 C44 H44 118.6 . . ?
C43 C44 C45 122.7(4) . . ?
C45 C44 H44 118.6 . . ?
C40 C45 C44 118.7(4) . . ?
C40 C45 H45 120.6 . . ?
C44 C45 H45 120.6 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C3 C2 C1 122.0(4) . . ?
C3 C2 C7 117.8(4) . . ?
C7 C2 C1 120.2(4) . . ?
C9 S3 C6 105.65(19) . . ?
C2 C3 H3 119.0 . . ?
C2 C3 C4 122.0(4) . . ?
C4 C3 H3 119.0 . . ?
O3 S4 O4 119.6(2) . . ?
O3 S4 C8 109.7(2) . . ?
O3 S4 C18 108.3(2) . . ?
O4 S4 C8 104.2(2) . . ?
O4 S4 C18 107.3(2) . . ?
C8 S4 C18 107.07(19) . . ?
C3 C4 H4 120.2 . . ?
C6 C4 C3 119.6(4) . . ?
C6 C4 H4 120.2 . . ?
C14 O5 C16 117.7(4) . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C7 120.3(4) . . ?
C7 C5 H5 119.9 . . ?
C4 C6 S3 120.2(3) . . ?
C4 C6 C5 119.1(4) . . ?
C5 C6 S3 120.3(3) . . ?
C2 C7 C5 121.2(4) . . ?
C2 C7 H7 119.4 . . ?
C5 C7 H7 119.4 . . ?
S4 C8 H8 116.9 . . ?
C9 C8 S4 126.1(3) . . ?
C9 C8 H8 116.9 . . ?
C8 C9 S3 124.5(3) . . ?
C8 C9 C10 126.4(4) . . ?
C10 C9 S3 109.1(3) . . ?
C11 C10 C9 120.3(3) . . ?
C12 C10 C9 121.3(3) . . ?
C12 C10 C11 118.3(4) . . ?
C10 C11 H11 119.5 . . ?
C15 C11 C10 121.0(4) . . ?
C15 C11 H11 119.5 . . ?
C10 C12 H12 119.2 . . ?
C10 C12 C13 121.7(4) . . ?
C13 C12 H12 119.2 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.3(4) . . ?
C14 C13 H13 120.4 . . ?
O5 C14 C13 124.9(4) . . ?
O5 C14 C15 115.8(4) . . ?
C13 C14 C15 119.4(4) . . ?
C11 C15 C14 120.4(4) . . ?
C11 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
O5 C16 H16A 109.5 . . ?
O5 C16 H16B 109.5 . . ?
O5 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 H17 120.2 . . ?
C22 C17 H17 120.2 . . ?
C22 C17 C18 119.7(5) . . ?
C17 C18 S4 120.5(3) . . ?
C19 C18 S4 120.0(3) . . ?
C19 C18 C17 119.6(4) . . ?
C18 C19 H19 120.1 . . ?
C18 C19 C20 119.7(4) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.5(5) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 C22 117.9(5) . . ?
C20 C21 C23 121.0(6) . . ?
C22 C21 C23 121.1(5) . . ?
C17 C22 C21 121.6(4) . . ?
C17 C22 H22 119.2 . . ?
C21 C22 H22 119.2 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Cl1 C47 Cl2 110.2(4) . . ?
Cl1 C47 Cl3 110.9(4) . . ?
Cl1 C47 H47 108.4 . . ?
Cl2 C47 H47 108.4 . . ?
Cl3 C47 Cl2 110.4(4) . . ?
Cl3 C47 H47 108.4 . . ?
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 C39 1.758(4) . ?
S1 C40 1.784(4) . ?
O1 S2 1.442(3) . ?
S2 O2 1.431(3) . ?
S2 C28 1.750(5) . ?
S2 C38 1.750(4) . ?
O6 C31 1.419(6) . ?
O6 C32 1.361(5) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 C25 1.517(8) . ?
C25 C26 1.386(8) . ?
C25 C30 1.373(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.367(8) . ?
C27 H27 0.9300 . ?
C27 C28 1.379(7) . ?
C28 C29 1.382(6) . ?
C29 H29 0.9300 . ?
C29 C30 1.385(7) . ?
C30 H30 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.374(6) . ?
C32 C37 1.382(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.394(6) . ?
C34 H34 0.9300 . ?
C34 C35 1.368(6) . ?
C35 C36 1.382(6) . ?
C35 C39 1.495(5) . ?
C36 H36 0.9300 . ?
C36 C37 1.377(6) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C38 C39 1.329(6) . ?
C40 C41 1.387(6) . ?
C40 C45 1.384(6) . ?
C41 H41 0.9300 . ?
C41 C42 1.372(6) . ?
C42 H42 0.9300 . ?
C42 C43 1.393(6) . ?
C43 C44 1.368(6) . ?
C43 C46 1.510(6) . ?
C44 H44 0.9300 . ?
C44 C45 1.389(6) . ?
C45 H45 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 C2 1.507(6) . ?
C2 C3 1.363(6) . ?
C2 C7 1.382(6) . ?
S3 C6 1.777(4) . ?
S3 C9 1.756(4) . ?
O3 S4 1.427(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.391(6) . ?
S4 O4 1.434(3) . ?
S4 C8 1.758(4) . ?
S4 C18 1.758(4) . ?
C4 H4 0.9300 . ?
C4 C6 1.378(6) . ?
O5 C14 1.361(5) . ?
O5 C16 1.415(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(6) . ?
C5 C7 1.384(6) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C8 C9 1.338(6) . ?
C9 C10 1.488(5) . ?
C10 C11 1.377(5) . ?
C10 C12 1.370(5) . ?
C11 H11 0.9300 . ?
C11 C15 1.363(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.383(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.374(6) . ?
C14 C15 1.387(6) . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17 0.9300 . ?
C17 C18 1.387(6) . ?
C17 C22 1.371(7) . ?
C18 C19 1.375(6) . ?
C19 H19 0.9300 . ?
C19 C20 1.379(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.376(7) . ?
C21 C22 1.380(8) . ?
C21 C23 1.517(7) . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
Cl1 C47 1.710(6) . ?
Cl2 C47 1.735(6) . ?
Cl3 C47 1.725(6) . ?
C47 H47 0.9800 . ?
