#------------------------------------------------------------------------------
#$Date: 2022-10-20 03:39:49 +0300 (Thu, 20 Oct 2022) $
#$Revision: 278643 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/15/89/7158944.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_7158944
loop_
_publ_author_name
'Hsueh, Nai-Chen'
'Chang, Meng-Yang'
_publ_section_title
;
 Tandem cyclocondensation of 1,3-bis-sulfonylpropan-2-ones with
 arylaldehydes. One-pot synthesis of tris-sulfonyl 3-arylphenols
;
_journal_name_full               'Organic & Biomolecular Chemistry'
_journal_paper_doi               10.1039/D2OB01703B
_journal_year                    2022
_chemical_formula_moiety         'C35 H32 O9 S3'
_chemical_formula_sum            'C35 H32 O9 S3'
_chemical_formula_weight         692.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-12-08
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.07.16 svn.r6f6c53a7 for OlexSys, GUI svn.r6139)
;
_audit_update_record
;
2020-12-08 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.673(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5860(3)
_cell_length_b                   12.8979(2)
_cell_length_c                   16.9919(3)
_cell_measurement_reflns_used    21454
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.9020
_cell_measurement_theta_min      2.1450
_cell_volume                     3151.85(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.56a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00 100.00   0.50   30.65    --   10.60  38.00   0.00  254
  2  ω    -20.00 100.00   0.50   30.65    --   10.60  57.00 -60.00  240
  3  ω    -17.00 100.00   0.50   30.65    --   10.60  82.00   0.00  234
  4  ω    -17.00 100.00   0.50   30.65    --   10.60  82.00  30.00  234
  5  ω    -15.00 100.00   0.50   30.65    --   10.60  77.00 -90.00  230
  6  ω    -41.00  75.00   0.50   30.65    --  -10.90  57.00-120.00  232
  7  ω    -54.00  19.00   0.50   30.65    --  -10.90 -57.00-120.00  146
  8  ω    -94.00 -61.00   0.50   30.65    --  -10.90 -57.00-120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro II AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0317394000
_diffrn_orient_matrix_UB_12      -0.0335325000
_diffrn_orient_matrix_UB_13      0.0081500000
_diffrn_orient_matrix_UB_21      -0.0193115000
_diffrn_orient_matrix_UB_22      0.0429573000
_diffrn_orient_matrix_UB_23      0.0134032000
_diffrn_orient_matrix_UB_31      -0.0324793000
_diffrn_orient_matrix_UB_32      0.0071859000
_diffrn_orient_matrix_UB_33      -0.0424291000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40771
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.56a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.437
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0897
_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)+(0.0586P)²+12.0123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2108
_refine_ls_wR_factor_ref         0.2145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4909
_reflns_number_total             5551
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ob01703b2.cif
_cod_data_source_block           k10912-myc-b
_cod_original_cell_volume        3151.85(10)
_cod_database_code               7158944
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid bond restraints
 C11, C14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 7.7
 C18, C21
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 12
3. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4.a Riding coordinates:
 O1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C10(H10), C12(H12), C13(H13), C16(H16), C17(H17), C19(H19),
 C20(H20), C23(H23), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C)
;
_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 1.148
_oxdiff_exptl_absorpt_empirical_full_min 0.880
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'
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 0.61827(13) -0.30203(15) 0.88061(13) 0.0745(6) Uani 1 1 d . . . . .
S2 S 0.64323(9) 0.01431(12) 0.80141(9) 0.0490(4) Uani 1 1 d . . . . .
S3 S 0.30317(9) 0.08536(11) 0.83042(8) 0.0423(3) Uani 1 1 d . . . . .
O1 O 0.3743(3) -0.0949(3) 0.9592(2) 0.0526(10) Uani 1 1 d . . . . .
H1 H 0.319310 -0.075808 0.931573 0.079 Uiso 1 1 d R U . . .
O2 O 0.5534(4) -0.3446(4) 0.9140(3) 0.0815(15) Uani 1 1 d . . . . .
O3 O 0.7035(4) -0.3571(5) 0.8965(4) 0.107(2) Uani 1 1 d . . . . .
O4 O 0.7312(3) -0.0152(4) 0.8656(3) 0.0778(15) Uani 1 1 d . . . . .
O5 O 0.6164(3) -0.0316(3) 0.7184(3) 0.0623(11) Uani 1 1 d . . . . .
O6 O 0.3828(3) 0.1259(3) 0.5170(2) 0.0465(9) Uani 1 1 d . . . . .
O7 O 0.3852(3) 0.3220(3) 0.5467(2) 0.0525(10) Uani 1 1 d . . . . .
O8 O 0.2499(3) 0.0297(3) 0.8712(3) 0.0561(10) Uani 1 1 d . . . . .
O9 O 0.3208(3) 0.1927(3) 0.8527(2) 0.0513(10) Uani 1 1 d . . . . .
C1 C 0.4285(4) -0.0655(4) 0.9178(3) 0.0421(12) Uani 1 1 d . . . . .
C2 C 0.5094(4) -0.1215(4) 0.9369(3) 0.0463(13) Uani 1 1 d . . . . .
H2 H 0.521969 -0.176448 0.977059 0.056 Uiso 1 1 calc R U . . .
C3 C 0.5725(4) -0.1016(4) 0.9007(3) 0.0449(12) Uani 1 1 d . . . . .
C4 C 0.5555(3) -0.0177(4) 0.8430(3) 0.0392(11) Uani 1 1 d . . . . .
C5 C 0.4727(3) 0.0389(4) 0.8193(3) 0.0348(10) Uani 1 1 d . . . . .
C6 C 0.4091(3) 0.0150(4) 0.8579(3) 0.0374(11) Uani 1 1 d . . . . .
C7 C 0.6526(4) -0.1763(5) 0.9232(4) 0.0652(18) Uani 1 1 d . . . . .
H7A H 0.683407 -0.181296 0.986007 0.078 Uiso 1 1 calc R U . . .
H7B H 0.698615 -0.148730 0.901473 0.078 Uiso 1 1 calc R U . . .
C8 C 0.5590(4) -0.2851(5) 0.7707(4) 0.0579(15) Uani 1 1 d . . . . .
C9 C 0.6090(5) -0.2805(6) 0.7193(5) 0.074(2) Uani 1 1 d . . . . .
H9 H 0.674894 -0.285132 0.742694 0.088 Uiso 1 1 calc R U . . .
C10 C 0.5603(5) -0.2689(6) 0.6331(5) 0.072(2) Uani 1 1 d . . . . .
H10 H 0.593381 -0.265641 0.596408 0.086 Uiso 1 1 calc R U . . .
C11 C 0.4657(5) -0.2619(6) 0.5988(5) 0.073(2) Uani 1 1 d . U . . .
C12 C 0.4169(5) -0.2627(6) 0.6521(5) 0.076(2) Uani 1 1 d . . . . .
H12 H 0.351295 -0.254551 0.628543 0.091 Uiso 1 1 calc R U . . .
C13 C 0.4624(5) -0.2749(5) 0.7375(5) 0.0662(18) Uani 1 1 d . . . . .
H13 H 0.429159 -0.276402 0.774054 0.079 Uiso 1 1 calc R U . . .
C14 C 0.4191(7) -0.2665(8) 0.5101(6) 0.106(3) Uani 1 1 d . U . . .
H14A H 0.393091 -0.336087 0.493566 0.159 Uiso 1 1 calc R U . . .
H14B H 0.462792 -0.251321 0.482854 0.159 Uiso 1 1 calc R U . . .
H14C H 0.368706 -0.215366 0.491825 0.159 Uiso 1 1 calc R U . . .
C15 C 0.6494(3) 0.1494(5) 0.7928(3) 0.0438(12) Uani 1 1 d . . . . .
C16 C 0.6330(3) 0.1912(5) 0.7131(3) 0.0459(13) Uani 1 1 d . . . . .
H16 H 0.614467 0.148769 0.663669 0.055 Uiso 1 1 calc R U . . .
C17 C 0.6446(4) 0.2974(5) 0.7084(5) 0.0634(17) Uani 1 1 d . . . . .
H17 H 0.635429 0.328373 0.655014 0.076 Uiso 1 1 calc R U . . .
C18 C 0.6692(5) 0.3585(6) 0.7805(6) 0.082(2) Uani 1 1 d . U . . .
C19 C 0.6874(5) 0.3144(7) 0.8590(5) 0.076(2) Uani 1 1 d . . . . .
H19 H 0.706121 0.356754 0.908576 0.091 Uiso 1 1 calc R U . . .
C20 C 0.6784(4) 0.2093(6) 0.8657(4) 0.0612(17) Uani 1 1 d . . . . .
H20 H 0.691925 0.178184 0.919861 0.073 Uiso 1 1 calc R U . . .
C21 C 0.6589(8) 0.4678(9) 0.7631(8) 0.131(3) Uani 1 1 d . U . . .
H21A H 0.601061 0.492090 0.767038 0.197 Uiso 1 1 calc R U . . .
H21B H 0.656745 0.481033 0.705618 0.197 Uiso 1 1 calc R U . . .
H21C H 0.711739 0.504847 0.804919 0.197 Uiso 1 1 calc R U . . .
C22 C 0.4483(3) 0.1187(4) 0.7502(3) 0.0323(10) Uani 1 1 d . . . . .
C23 C 0.4246(3) 0.0831(4) 0.6665(3) 0.0335(10) Uani 1 1 d . . . . .
H23 H 0.423029 0.010814 0.655308 0.040 Uiso 1 1 calc R U . . .
C24 C 0.4033(3) 0.1536(4) 0.6003(3) 0.0348(10) Uani 1 1 d . . . . .
C25 C 0.4052(3) 0.2595(4) 0.6167(3) 0.0391(11) Uani 1 1 d . . . . .
C26 C 0.4267(3) 0.2944(4) 0.6985(3) 0.0404(11) Uani 1 1 d . . . . .
H26 H 0.426817 0.366625 0.709379 0.048 Uiso 1 1 calc R U . . .
C27 C 0.4482(3) 0.2239(4) 0.7654(3) 0.0382(11) Uani 1 1 d . . . . .
H27 H 0.462793 0.248260 0.821882 0.046 Uiso 1 1 calc R U . . .
C28 C 0.3791(4) 0.0185(5) 0.4981(3) 0.0526(14) Uani 1 1 d . . . . .
H28A H 0.438581 -0.013880 0.532857 0.079 Uiso 1 1 calc R U . . .
H28B H 0.367209 0.009145 0.437509 0.079 Uiso 1 1 calc R U . . .
H28C H 0.329044 -0.013999 0.510723 0.079 Uiso 1 1 calc R U . . .
C29 C 0.4072(4) 0.4297(4) 0.5599(4) 0.0583(16) Uani 1 1 d . . . . .
H29A H 0.369444 0.461695 0.588008 0.087 Uiso 1 1 calc R U . . .
H29B H 0.394001 0.463554 0.504842 0.087 Uiso 1 1 calc R U . . .
H29C H 0.473266 0.437901 0.596038 0.087 Uiso 1 1 calc R U . . .
C30 C 0.2151(4) -0.0261(5) 0.6867(4) 0.0551(15) Uani 1 1 d . . . . .
H30 H 0.232313 -0.085414 0.722627 0.066 Uiso 1 1 calc R U . . .
C31 C 0.1624(5) -0.0363(6) 0.5999(4) 0.078(2) Uani 1 1 d . . . . .
H31 H 0.143557 -0.103262 0.576160 0.094 Uiso 1 1 calc R U . . .
C32 C 0.1373(5) 0.0502(6) 0.5477(4) 0.075(2) Uani 1 1 d . . . . .
H32 H 0.100974 0.042918 0.488494 0.090 Uiso 1 1 calc R U . . .
C33 C 0.1651(4) 0.1457(5) 0.5821(4) 0.0582(17) Uani 1 1 d . . . . .
H33 H 0.148023 0.204792 0.545972 0.070 Uiso 1 1 calc R U . . .
C34 C 0.2174(4) 0.1592(4) 0.6681(4) 0.0479(13) Uani 1 1 d . . . . .
H34 H 0.236112 0.226427 0.691193 0.058 Uiso 1 1 calc R U . . .
C35 C 0.2419(3) 0.0722(4) 0.7198(3) 0.0392(11) Uani 1 1 d . . . . .
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'
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
O2 S1 C7 109.6(3) . . ?
O2 S1 C8 107.8(3) . . ?
O3 S1 O2 118.4(3) . . ?
O3 S1 C7 105.3(4) . . ?
O3 S1 C8 109.4(3) . . ?
C8 S1 C7 105.9(3) . . ?
O4 S2 C4 106.6(2) . . ?
O4 S2 C15 105.0(3) . . ?
O5 S2 O4 117.9(3) . . ?
O5 S2 C4 108.2(2) . . ?
O5 S2 C15 109.4(3) . . ?
C15 S2 C4 109.4(2) . . ?
O8 S3 C6 105.3(2) . . ?
O8 S3 C35 106.6(2) . . ?
O9 S3 O8 115.8(2) . . ?
O9 S3 C6 111.0(2) . . ?
O9 S3 C35 110.2(2) . . ?
C35 S3 C6 107.3(2) . . ?
C1 O1 H1 109.7 . . ?
C24 O6 C28 117.5(4) . . ?
C25 O7 C29 118.4(4) . . ?
O1 C1 C2 115.5(5) . . ?
O1 C1 C6 125.7(5) . . ?
C2 C1 C6 118.8(4) . . ?
C1 C2 H2 118.5 . . ?
C3 C2 C1 123.0(5) . . ?
C3 C2 H2 118.5 . . ?
C2 C3 C4 118.6(5) . . ?
C2 C3 C7 115.8(5) . . ?
C4 C3 C7 125.5(5) . . ?
C3 C4 S2 118.5(4) . . ?
C5 C4 S2 121.3(4) . . ?
C5 C4 C3 120.2(4) . . ?
C4 C5 C6 119.0(4) . . ?
C4 C5 C22 120.8(4) . . ?
C6 C5 C22 120.1(4) . . ?
C1 C6 S3 119.2(4) . . ?
C1 C6 C5 120.1(5) . . ?
C5 C6 S3 120.7(4) . . ?
S1 C7 H7A 109.0 . . ?
S1 C7 H7B 109.0 . . ?
C3 C7 S1 113.1(4) . . ?
C3 C7 H7A 109.0 . . ?
C3 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C9 C8 S1 119.2(5) . . ?
C9 C8 C13 121.7(7) . . ?
C13 C8 S1 119.2(5) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 C8 117.8(6) . . ?
C10 C9 H9 121.1 . . ?
C9 C10 H10 119.2 . . ?
C11 C10 C9 121.6(6) . . ?
C11 C10 H10 119.2 . . ?
C10 C11 C12 119.7(7) . . ?
C10 C11 C14 119.0(7) . . ?
C12 C11 C14 120.9(8) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.4(7) . . ?
C13 C12 H12 119.8 . . ?
C8 C13 H13 120.6 . . ?
C12 C13 C8 118.7(6) . . ?
C12 C13 H13 120.6 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 S2 118.2(4) . . ?
C20 C15 S2 119.4(5) . . ?
C20 C15 C16 122.1(6) . . ?
C15 C16 H16 121.3 . . ?
C15 C16 C17 117.5(6) . . ?
C17 C16 H16 121.3 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.6(7) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 C21 114.0(9) . . ?
C19 C18 C17 120.5(7) . . ?
C19 C18 C21 124.7(9) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 119.9(7) . . ?
C20 C19 H19 120.0 . . ?
C15 C20 H20 120.4 . . ?
C19 C20 C15 119.2(6) . . ?
C19 C20 H20 120.4 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C5 117.4(4) . . ?
C27 C22 C5 123.1(4) . . ?
C27 C22 C23 119.5(4) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 H23 120.1 . . ?
O6 C24 C23 123.7(5) . . ?
O6 C24 C25 116.1(4) . . ?
C23 C24 C25 120.1(4) . . ?
O7 C25 C24 115.1(4) . . ?
O7 C25 C26 124.8(5) . . ?
C26 C25 C24 120.1(4) . . ?
C25 C26 H26 120.0 . . ?
C25 C26 C27 120.1(5) . . ?
C27 C26 H26 120.0 . . ?
C22 C27 C26 120.4(4) . . ?
C22 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O7 C29 H29A 109.5 . . ?
O7 C29 H29B 109.5 . . ?
O7 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 H30 120.7 . . ?
C35 C30 H30 120.7 . . ?
C35 C30 C31 118.7(6) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 C30 120.6(7) . . ?
C32 C31 H31 119.7 . . ?
C31 C32 H32 120.3 . . ?
C33 C32 C31 119.4(6) . . ?
C33 C32 H32 120.3 . . ?
C32 C33 H33 119.1 . . ?
C32 C33 C34 121.9(6) . . ?
C34 C33 H33 119.1 . . ?
C33 C34 H34 120.8 . . ?
C33 C34 C35 118.3(6) . . ?
C35 C34 H34 120.8 . . ?
C30 C35 S3 118.5(4) . . ?
C30 C35 C34 121.2(5) . . ?
C34 C35 S3 120.2(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 O2 1.445(5) . ?
S1 O3 1.437(5) . ?
S1 C7 1.772(8) . ?
S1 C8 1.749(7) . ?
S2 O4 1.435(4) . ?
S2 O5 1.435(4) . ?
S2 C4 1.812(5) . ?
S2 C15 1.754(6) . ?
S3 O8 1.459(4) . ?
S3 O9 1.434(4) . ?
S3 C6 1.780(5) . ?
S3 C35 1.757(5) . ?
O1 H1 0.8400 . ?
O1 C1 1.346(6) . ?
O6 C24 1.372(5) . ?
O6 C28 1.419(7) . ?
O7 C25 1.369(6) . ?
O7 C29 1.428(7) . ?
C1 C2 1.378(8) . ?
C1 C6 1.403(7) . ?
C2 H2 0.9500 . ?
C2 C3 1.371(7) . ?
C3 C4 1.415(7) . ?
C3 C7 1.505(8) . ?
C4 C5 1.400(7) . ?
C5 C6 1.418(6) . ?
C5 C22 1.496(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.378(8) . ?
C8 C13 1.395(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.374(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.363(10) . ?
C11 C12 1.388(9) . ?
C11 C14 1.400(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.357(10) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.387(7) . ?
C15 C20 1.380(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.381(10) . ?
C18 C19 1.376(11) . ?
C18 C21 1.436(13) . ?
C19 H19 0.9500 . ?
C19 C20 1.373(10) . ?
C20 H20 0.9500 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.401(6) . ?
C22 C27 1.382(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(6) . ?
C24 C25 1.392(7) . ?
C25 C26 1.374(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.392(7) . ?
C27 H27 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30 0.9500 . ?
C30 C31 1.391(9) . ?
C30 C35 1.385(8) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.361(10) . ?
C33 H33 0.9500 . ?
C33 C34 1.384(8) . ?
C34 H34 0.9500 . ?
C34 C35 1.385(7) . ?
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
S1 C8 C9 C10 178.9(6) . . . . ?
S1 C8 C13 C12 -179.4(6) . . . . ?
S2 C4 C5 C6 -175.9(4) . . . . ?
S2 C4 C5 C22 8.2(6) . . . . ?
S2 C15 C16 C17 -175.5(4) . . . . ?
S2 C15 C20 C19 176.9(5) . . . . ?
O1 C1 C2 C3 -179.8(5) . . . . ?
O1 C1 C6 S3 -1.4(7) . . . . ?
O1 C1 C6 C5 179.3(5) . . . . ?
O2 S1 C7 C3 -60.6(5) . . . . ?
O2 S1 C8 C9 -157.6(6) . . . . ?
O2 S1 C8 C13 23.4(6) . . . . ?
O3 S1 C7 C3 171.1(4) . . . . ?
O3 S1 C8 C9 -27.7(7) . . . . ?
O3 S1 C8 C13 153.3(6) . . . . ?
O4 S2 C4 C3 -29.3(5) . . . . ?
O4 S2 C4 C5 150.5(4) . . . . ?
O4 S2 C15 C16 124.7(4) . . . . ?
O4 S2 C15 C20 -49.4(5) . . . . ?
O5 S2 C4 C3 98.5(4) . . . . ?
O5 S2 C4 C5 -81.8(5) . . . . ?
O5 S2 C15 C16 -2.8(5) . . . . ?
O5 S2 C15 C20 -176.9(4) . . . . ?
O6 C24 C25 O7 0.6(6) . . . . ?
O6 C24 C25 C26 -178.9(4) . . . . ?
O7 C25 C26 C27 -178.4(4) . . . . ?
O8 S3 C6 C1 -8.1(5) . . . . ?
O8 S3 C6 C5 171.2(4) . . . . ?
O8 S3 C35 C30 -50.8(5) . . . . ?
O8 S3 C35 C34 126.1(4) . . . . ?
O9 S3 C6 C1 118.0(4) . . . . ?
O9 S3 C6 C5 -62.7(4) . . . . ?
O9 S3 C35 C30 -177.3(4) . . . . ?
O9 S3 C35 C34 -0.4(5) . . . . ?
C1 C2 C3 C4 2.0(8) . . . . ?
C1 C2 C3 C7 -174.8(5) . . . . ?
C2 C1 C6 S3 178.2(4) . . . . ?
C2 C1 C6 C5 -1.1(7) . . . . ?
C2 C3 C4 S2 175.5(4) . . . . ?
C2 C3 C4 C5 -4.3(8) . . . . ?
C2 C3 C7 S1 67.6(6) . . . . ?
C3 C4 C5 C6 3.8(7) . . . . ?
C3 C4 C5 C22 -172.1(5) . . . . ?
C4 S2 C15 C16 -121.1(4) . . . . ?
C4 S2 C15 C20 64.7(5) . . . . ?
C4 C3 C7 S1 -108.9(6) . . . . ?
C4 C5 C6 S3 179.6(4) . . . . ?
C4 C5 C6 C1 -1.1(7) . . . . ?
C4 C5 C22 C23 70.0(6) . . . . ?
C4 C5 C22 C27 -110.1(5) . . . . ?
C5 C22 C23 C24 -178.6(4) . . . . ?
C5 C22 C27 C26 178.7(4) . . . . ?
C6 S3 C35 C30 61.7(5) . . . . ?
C6 S3 C35 C34 -121.4(4) . . . . ?
C6 C1 C2 C3 0.6(8) . . . . ?
C6 C5 C22 C23 -105.8(5) . . . . ?
C6 C5 C22 C27 74.0(6) . . . . ?
C7 S1 C8 C9 85.2(6) . . . . ?
C7 S1 C8 C13 -93.7(6) . . . . ?
C7 C3 C4 S2 -8.0(8) . . . . ?
C7 C3 C4 C5 172.2(5) . . . . ?
C8 S1 C7 C3 55.4(5) . . . . ?
C8 C9 C10 C11 0.1(11) . . . . ?
C9 C8 C13 C12 1.7(10) . . . . ?
C9 C10 C11 C12 2.4(12) . . . . ?
C9 C10 C11 C14 -170.1(8) . . . . ?
C10 C11 C12 C13 -3.0(12) . . . . ?
C11 C12 C13 C8 0.9(11) . . . . ?
C13 C8 C9 C10 -2.2(11) . . . . ?
C14 C11 C12 C13 169.5(8) . . . . ?
C15 S2 C4 C3 -142.4(4) . . . . ?
C15 S2 C4 C5 37.3(5) . . . . ?
C15 C16 C17 C18 -1.6(8) . . . . ?
C16 C15 C20 C19 3.0(8) . . . . ?
C16 C17 C18 C19 3.3(10) . . . . ?
C16 C17 C18 C21 -167.1(7) . . . . ?
C17 C18 C19 C20 -1.9(10) . . . . ?
C18 C19 C20 C15 -1.2(9) . . . . ?
C20 C15 C16 C17 -1.5(7) . . . . ?
C21 C18 C19 C20 167.5(8) . . . . ?
C22 C5 C6 S3 -4.5(6) . . . . ?
C22 C5 C6 C1 174.8(4) . . . . ?
C22 C23 C24 O6 177.4(4) . . . . ?
C22 C23 C24 C25 -0.2(7) . . . . ?
C23 C22 C27 C26 -1.5(7) . . . . ?
C23 C24 C25 O7 178.5(4) . . . . ?
C23 C24 C25 C26 -1.1(7) . . . . ?
C24 C25 C26 C27 1.1(7) . . . . ?
C25 C26 C27 C22 0.2(7) . . . . ?
C27 C22 C23 C24 1.5(6) . . . . ?
C28 O6 C24 C23 3.0(7) . . . . ?
C28 O6 C24 C25 -179.2(4) . . . . ?
C29 O7 C25 C24 -165.1(4) . . . . ?
C29 O7 C25 C26 14.4(7) . . . . ?
C30 C31 C32 C33 0.4(11) . . . . ?
C31 C30 C35 S3 176.7(5) . . . . ?
C31 C30 C35 C34 -0.2(9) . . . . ?
C31 C32 C33 C34 -0.5(10) . . . . ?
C32 C33 C34 C35 0.2(8) . . . . ?
C33 C34 C35 S3 -176.7(4) . . . . ?
C33 C34 C35 C30 0.1(7) . . . . ?
C35 S3 C6 C1 -121.4(4) . . . . ?
C35 S3 C6 C5 57.8(5) . . . . ?
C35 C30 C31 C32 -0.1(11) . . . . ?
