#------------------------------------------------------------------------------
#$Date: 2023-05-05 02:33:52 +0200 (Fri 05 de May de 2023) $
#$Revision: 283117 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/14/7131496.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_7131496
loop_
_publ_author_name
'Gupta, Anish'
'Jandial, Tanvi'
'Karuppasamy, Muthu'
'Bhuvanesh, Nattamai'
'Nagarajan, Subbiah'
'Maheswari, C. Uma'
'Sridharan, Vellaisamy'
_publ_section_title
;
 Palladium-catalyzed intramolecular oxypalladation-initiated cascade:
 solvent-dependent chemodivergent approach to functionalized benzazepines
 and tetrahydroquinolines.
;
_journal_issue                   35
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5233
_journal_page_last               5236
_journal_paper_doi               10.1039/d3cc01370g
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C32 H25 N O5 S, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C34 H29 N O6 S'
_chemical_formula_weight         579.64
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-22 deposited with the CCDC.	2023-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90.682(2)
_cell_angle_beta                 99.416(2)
_cell_angle_gamma                97.172(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5669(6)
_cell_length_b                   11.3682(6)
_cell_length_c                   11.9934(6)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    110.00
_cell_measurement_theta_max      29.524
_cell_measurement_theta_min      2.392
_cell_volume                     1409.43(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      110.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Quest (PHOTON III)'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            46933
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.914
_diffrn_reflns_theta_min         1.806
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0855 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.9639.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8098
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0758P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6023
_reflns_number_total             8098
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc01370g2.cif
_cod_data_source_block           ag134
_cod_depositor_comments          'Adding full bibliography for 7131496.cif.'
_cod_database_code               7131496
_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.
;
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.967
_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
2. Uiso/Uaniso restraints and constraints
O1S \\sim O2S \\sim C1S \\sim C2S \\sim C3S \\sim C4S: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 O1S, O2S, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Others
 Fixed Sof: O1S(0.5) O2S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5)
 C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) H4SC(0.5)
5.a Ternary CH refined with riding coordinates:
 C4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C25(H25A,H25B), C3S(H3SA,H3SB)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C28(H28), C29(H29), C30(H30),
  C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_olex2_submission_special_instructions 'No special instructions were received'
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 0.55896(3) 0.73688(3) 0.03525(3) 0.02037(9) Uani 1 1 d . . . . .
O1 O 0.44416(9) 0.44591(7) 0.29546(7) 0.0229(2) Uani 1 1 d . . . . .
O2 O 0.39988(10) 0.27789(8) 0.37945(8) 0.0320(2) Uani 1 1 d . . . . .
O3 O 0.63978(9) 0.84821(8) 0.03877(8) 0.0267(2) Uani 1 1 d . . . . .
O4 O 0.60667(9) 0.62878(8) 0.00855(8) 0.0267(2) Uani 1 1 d . . . . .
O5 O 0.94728(10) 0.84031(10) 0.43969(8) 0.0388(3) Uani 1 1 d . . . . .
N1 N 0.52031(11) 0.72303(9) 0.16110(9) 0.0221(2) Uani 1 1 d . . . . .
C1 C 0.44803(12) 0.61365(11) 0.19026(10) 0.0223(3) Uani 1 1 d . . . . .
H1A H 0.428570 0.558532 0.123387 0.027 Uiso 1 1 calc R U . . .
H1B H 0.364665 0.631447 0.209498 0.027 Uiso 1 1 calc R U . . .
C2 C 0.51875(12) 0.55335(10) 0.28779(10) 0.0196(2) Uani 1 1 d . . . . .
C3 C 0.62986(12) 0.58859(10) 0.35772(10) 0.0195(3) Uani 1 1 d . . . . .
C4 C 0.70835(12) 0.71111(10) 0.36168(10) 0.0212(3) Uani 1 1 d . . . . .
H4 H 0.752935 0.724072 0.441884 0.025 Uiso 1 1 calc R U . . .
C5 C 0.63141(12) 0.81466(11) 0.33880(11) 0.0216(3) Uani 1 1 d . . . . .
C6 C 0.54114(13) 0.82138(11) 0.24145(11) 0.0235(3) Uani 1 1 d . . . . .
C7 C 0.47586(13) 0.36612(11) 0.37690(11) 0.0232(3) Uani 1 1 d . . . . .
C8 C 0.60040(13) 0.39578(11) 0.45052(11) 0.0223(3) Uani 1 1 d . . . . .
C9 C 0.67753(12) 0.50369(11) 0.44001(10) 0.0215(3) Uani 1 1 d . . . . .
C10 C 0.64113(14) 0.31367(11) 0.53058(12) 0.0278(3) Uani 1 1 d . . . . .
H10 H 0.586353 0.242257 0.537838 0.033 Uiso 1 1 calc R U . . .
C11 C 0.75997(15) 0.33609(13) 0.59856(12) 0.0329(3) Uani 1 1 d . . . . .
H11 H 0.787844 0.280569 0.652851 0.040 Uiso 1 1 calc R U . . .
C12 C 0.83904(14) 0.44116(14) 0.58691(13) 0.0341(3) Uani 1 1 d . . . . .
H12 H 0.922214 0.455838 0.632417 0.041 Uiso 1 1 calc R U . . .
C13 C 0.79927(13) 0.52433(12) 0.51081(12) 0.0283(3) Uani 1 1 d . . . . .
H13 H 0.854253 0.596213 0.505921 0.034 Uiso 1 1 calc R U . . .
C14 C 0.65270(14) 0.90965(11) 0.41686(11) 0.0275(3) Uani 1 1 d . . . . .
H14 H 0.713544 0.907510 0.484304 0.033 Uiso 1 1 calc R U . . .
C15 C 0.58664(16) 1.00700(12) 0.39772(13) 0.0354(4) Uani 1 1 d . . . . .
H15 H 0.605371 1.072478 0.450324 0.042 Uiso 1 1 calc R U . . .
C16 C 0.49314(16) 1.00982(13) 0.30219(14) 0.0381(4) Uani 1 1 d . . . . .
H16 H 0.445739 1.075581 0.290479 0.046 Uiso 1 1 calc R U . . .
C17 C 0.46983(15) 0.91555(12) 0.22418(13) 0.0313(3) Uani 1 1 d . . . . .
H17 H 0.405119 0.915604 0.159082 0.038 Uiso 1 1 calc R U . . .
C18 C 0.41676(12) 0.74412(11) -0.06275(10) 0.0199(2) Uani 1 1 d . . . . .
C19 C 0.37300(13) 0.85281(11) -0.08627(11) 0.0251(3) Uani 1 1 d . . . . .
H19 H 0.415155 0.922584 -0.045032 0.030 Uiso 1 1 calc R U . . .
C20 C 0.26780(13) 0.85865(12) -0.17001(11) 0.0277(3) Uani 1 1 d . . . . .
H20 H 0.238017 0.933060 -0.186149 0.033 Uiso 1 1 calc R U . . .
C21 C 0.20448(13) 0.75734(12) -0.23132(11) 0.0271(3) Uani 1 1 d . . . . .
C22 C 0.24747(13) 0.64929(12) -0.20341(12) 0.0284(3) Uani 1 1 d . . . . .
H22 H 0.203427 0.579071 -0.242715 0.034 Uiso 1 1 calc R U . . .
C23 C 0.35276(13) 0.64118(11) -0.11987(11) 0.0238(3) Uani 1 1 d . . . . .
H23 H 0.380805 0.566447 -0.101878 0.029 Uiso 1 1 calc R U . . .
C24 C 0.09548(15) 0.76507(15) -0.32804(13) 0.0408(4) Uani 1 1 d . . . . .
H24A H 0.082441 0.692780 -0.376043 0.061 Uiso 1 1 calc R U . . .
H24B H 0.117120 0.834026 -0.372807 0.061 Uiso 1 1 calc R U . . .
H24C H 0.015999 0.773451 -0.298175 0.061 Uiso 1 1 calc R U . . .
C25 C 0.81830(12) 0.71749(11) 0.29116(11) 0.0228(3) Uani 1 1 d . . . . .
H25A H 0.852451 0.640217 0.292010 0.027 Uiso 1 1 calc R U . . .
H25B H 0.784189 0.733868 0.211758 0.027 Uiso 1 1 calc R U . . .
C26 C 0.92725(12) 0.81498(11) 0.33885(11) 0.0230(3) Uani 1 1 d . . . . .
C27 C 1.00756(12) 0.87816(12) 0.26172(12) 0.0241(3) Uani 1 1 d . . . . .
C28 C 1.08301(13) 0.98477(12) 0.30220(13) 0.0305(3) Uani 1 1 d . . . . .
H28 H 1.082974 1.013516 0.376899 0.037 Uiso 1 1 calc R U . . .
C29 C 1.15758(15) 1.04813(15) 0.23321(16) 0.0446(4) Uani 1 1 d . . . . .
H29 H 1.207788 1.121151 0.260149 0.053 Uiso 1 1 calc R U . . .
C30 C 1.15928(16) 1.00582(19) 0.12591(17) 0.0581(6) Uani 1 1 d . . . . .
H30 H 1.210235 1.049927 0.078608 0.070 Uiso 1 1 calc R U . . .
C31 C 1.08694(16) 0.8990(2) 0.08628(15) 0.0589(6) Uani 1 1 d . . . . .
H31 H 1.090006 0.868966 0.012632 0.071 Uiso 1 1 calc R U . . .
C32 C 1.01025(14) 0.83609(16) 0.15413(13) 0.0395(4) Uani 1 1 d . . . . .
H32 H 0.959309 0.763676 0.126377 0.047 Uiso 1 1 calc R U . . .
O1S O 0.9763(3) 0.4517(2) -0.1527(2) 0.0585(7) Uani 0.5 1 d . U P A -1
O2S O 1.0226(2) 0.5533(2) 0.0118(2) 0.0498(6) Uani 0.5 1 d . U P A -1
C1S C 0.8636(4) 0.6181(5) -0.1264(5) 0.0471(11) Uani 0.5 1 d . U P A -1
H1SA H 0.796843 0.608612 -0.078135 0.071 Uiso 0.5 1 calc R U P A -1
H1SB H 0.823208 0.603008 -0.205623 0.071 Uiso 0.5 1 calc R U P A -1
H1SC H 0.908863 0.699170 -0.116698 0.071 Uiso 0.5 1 calc R U P A -1
C2S C 0.9586(3) 0.5316(3) -0.0936(3) 0.0371(7) Uani 0.5 1 d . U P A -1
C3S C 1.1230(4) 0.4796(4) 0.0512(4) 0.0683(11) Uani 0.5 1 d . U P A -1
H3SA H 1.158535 0.452017 -0.014398 0.082 Uiso 0.5 1 calc R U P A -1
H3SB H 1.194185 0.527948 0.102220 0.082 Uiso 0.5 1 calc R U P A -1
C4S C 1.0756(6) 0.3781(6) 0.1105(5) 0.0704(15) Uani 0.5 1 d . U P A -1
H4SA H 1.146256 0.331167 0.134947 0.106 Uiso 0.5 1 calc R U P A -1
H4SB H 1.005976 0.329275 0.060016 0.106 Uiso 0.5 1 calc R U P A -1
H4SC H 1.042359 0.404995 0.176739 0.106 Uiso 0.5 1 calc R U P A -1
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'
N N 0.0061 0.0033 '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
O3 S1 O4 120.37(6) . . ?
O3 S1 N1 105.74(5) . . ?
O3 S1 C18 108.69(6) . . ?
O4 S1 N1 106.68(5) . . ?
O4 S1 C18 106.45(6) . . ?
N1 S1 C18 108.46(6) . . ?
C7 O1 C2 123.02(10) . . ?
C1 N1 S1 120.19(8) . . ?
C6 N1 S1 121.93(8) . . ?
C6 N1 C1 117.42(10) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
N1 C1 C2 113.34(10) . . ?
H1A C1 H1B 107.7 . . ?
C2 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
O1 C2 C1 105.65(10) . . ?
C3 C2 O1 123.34(11) . . ?
C3 C2 C1 131.02(11) . . ?
C2 C3 C4 125.57(11) . . ?
C2 C3 C9 117.17(11) . . ?
C9 C3 C4 117.22(10) . . ?
C3 C4 H4 105.0 . . ?
C3 C4 C25 113.44(10) . . ?
C5 C4 C3 116.17(10) . . ?
C5 C4 H4 105.0 . . ?
C5 C4 C25 111.06(10) . . ?
C25 C4 H4 105.0 . . ?
C6 C5 C4 123.14(11) . . ?
C6 C5 C14 117.53(12) . . ?
C14 C5 C4 119.31(12) . . ?
C5 C6 N1 117.09(11) . . ?
C17 C6 N1 120.97(12) . . ?
C17 C6 C5 121.88(12) . . ?
O1 C7 C8 116.09(10) . . ?
O2 C7 O1 117.34(12) . . ?
O2 C7 C8 126.55(12) . . ?
C9 C8 C7 120.38(11) . . ?
C10 C8 C7 118.38(11) . . ?
C10 C8 C9 121.23(12) . . ?
C8 C9 C3 119.56(11) . . ?
C8 C9 C13 117.30(11) . . ?
C13 C9 C3 123.13(11) . . ?
C8 C10 H10 119.9 . . ?
C11 C10 C8 120.24(13) . . ?
C11 C10 H10 119.9 . . ?
C10 C11 H11 120.4 . . ?
C10 C11 C12 119.17(12) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.3 . . ?
C13 C12 C11 121.42(13) . . ?
C13 C12 H12 119.3 . . ?
C9 C13 H13 119.7 . . ?
C12 C13 C9 120.59(13) . . ?
C12 C13 H13 119.7 . . ?
C5 C14 H14 119.5 . . ?
C15 C14 C5 121.02(13) . . ?
C15 C14 H14 119.5 . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.51(13) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.19(14) . . ?
C17 C16 H16 120.4 . . ?
C6 C17 C16 119.73(14) . . ?
C6 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 S1 120.03(10) . . ?
C23 C18 S1 119.35(9) . . ?
C23 C18 C19 120.55(12) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.46(12) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.4 . . ?
C19 C20 C21 121.16(12) . . ?
C21 C20 H20 119.4 . . ?
C20 C21 C24 121.07(12) . . ?
C22 C21 C20 118.15(12) . . ?
C22 C21 C24 120.74(13) . . ?
C21 C22 H22 119.1 . . ?
C23 C22 C21 121.72(12) . . ?
C23 C22 H22 119.1 . . ?
C18 C23 H23 120.6 . . ?
C22 C23 C18 118.88(12) . . ?
C22 C23 H23 120.6 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C4 C25 H25A 109.5 . . ?
C4 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C26 C25 C4 110.51(10) . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
O5 C26 C25 119.60(12) . . ?
O5 C26 C27 120.70(12) . . ?
C27 C26 C25 119.70(11) . . ?
C28 C27 C26 117.48(13) . . ?
C32 C27 C26 122.88(13) . . ?
C32 C27 C28 119.63(13) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.82(15) . . ?
C29 C28 H28 120.1 . . ?
C28 C29 H29 119.9 . . ?
C30 C29 C28 120.16(16) . . ?
C30 C29 H29 119.9 . . ?
C29 C30 H30 119.9 . . ?
C29 C30 C31 120.25(16) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 119.91(18) . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 120.20(16) . . ?
C27 C32 H32 119.9 . . ?
C31 C32 H32 119.9 . . ?
C2S O2S C3S 117.0(3) . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
O1S C2S O2S 122.9(3) . . ?
O1S C2S C1S 125.3(4) . . ?
O2S C2S C1S 111.8(3) . . ?
O2S C3S H3SA 109.1 . . ?
O2S C3S H3SB 109.1 . . ?
H3SA C3S H3SB 107.8 . . ?
C4S C3S O2S 112.5(4) . . ?
C4S C3S H3SA 109.1 . . ?
C4S C3S H3SB 109.1 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
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 O3 1.4317(9) . ?
S1 O4 1.4371(9) . ?
S1 N1 1.6313(11) . ?
S1 C18 1.7611(13) . ?
O1 C2 1.3811(14) . ?
O1 C7 1.3707(15) . ?
O2 C7 1.2080(15) . ?
O5 C26 1.2178(16) . ?
N1 C1 1.4534(15) . ?
N1 C6 1.4390(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.5025(17) . ?
C2 C3 1.3397(17) . ?
C3 C4 1.5255(16) . ?
C3 C9 1.4631(17) . ?
C4 H4 1.0000 . ?
C4 C5 1.5151(17) . ?
C4 C25 1.5403(18) . ?
C5 C6 1.3910(18) . ?
C5 C14 1.3926(17) . ?
C6 C17 1.3830(18) . ?
C7 C8 1.4584(19) . ?
C8 C9 1.4046(17) . ?
C8 C10 1.4018(17) . ?
C9 C13 1.4119(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.374(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.392(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.3776(19) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.382(2) . ?
C15 H15 0.9500 . ?
C15 C16 1.389(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.385(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.3888(17) . ?
C18 C23 1.3884(17) . ?
C19 H19 0.9500 . ?
C19 C20 1.3796(18) . ?
C20 H20 0.9500 . ?
C20 C21 1.3933(19) . ?
C21 C22 1.3880(19) . ?
C21 C24 1.5068(19) . ?
C22 H22 0.9500 . ?
C22 C23 1.3832(18) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.5270(17) . ?
C26 C27 1.4873(18) . ?
C27 C28 1.3995(19) . ?
C27 C32 1.377(2) . ?
C28 H28 0.9500 . ?
C28 C29 1.382(2) . ?
C29 H29 0.9500 . ?
C29 C30 1.372(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.386(3) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(2) . ?
C32 H32 0.9500 . ?
O1S C2S 1.196(4) . ?
O2S C2S 1.338(4) . ?
O2S C3S 1.455(5) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.502(6) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.441(8) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
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 N1 C1 C2 119.84(10) . . . . ?
S1 N1 C6 C5 -114.07(12) . . . . ?
S1 N1 C6 C17 68.75(16) . . . . ?
S1 C18 C19 C20 174.57(10) . . . . ?
S1 C18 C23 C22 -174.65(10) . . . . ?
O1 C2 C3 C4 -172.85(11) . . . . ?
O1 C2 C3 C9 4.82(18) . . . . ?
O1 C7 C8 C9 3.30(17) . . . . ?
O1 C7 C8 C10 -176.06(11) . . . . ?
O2 C7 C8 C9 -178.15(13) . . . . ?
O2 C7 C8 C10 2.5(2) . . . . ?
O3 S1 N1 C1 -174.15(9) . . . . ?
O3 S1 N1 C6 13.81(12) . . . . ?
O3 S1 C18 C19 -26.18(12) . . . . ?
O3 S1 C18 C23 150.77(10) . . . . ?
O4 S1 N1 C1 -44.89(11) . . . . ?
O4 S1 N1 C6 143.07(10) . . . . ?
O4 S1 C18 C19 -157.20(10) . . . . ?
O4 S1 C18 C23 19.75(12) . . . . ?
O5 C26 C27 C28 -15.60(19) . . . . ?
O5 C26 C27 C32 164.32(14) . . . . ?
N1 S1 C18 C19 88.33(11) . . . . ?
N1 S1 C18 C23 -94.71(11) . . . . ?
N1 C1 C2 O1 -173.27(10) . . . . ?
N1 C1 C2 C3 7.1(2) . . . . ?
N1 C6 C17 C16 -179.14(13) . . . . ?
C1 N1 C6 C5 73.69(15) . . . . ?
C1 N1 C6 C17 -103.50(14) . . . . ?
C1 C2 C3 C4 6.8(2) . . . . ?
C1 C2 C3 C9 -175.56(12) . . . . ?
C2 O1 C7 O2 175.98(11) . . . . ?
C2 O1 C7 C8 -5.33(17) . . . . ?
C2 C3 C4 C5 35.13(17) . . . . ?
C2 C3 C4 C25 -95.37(15) . . . . ?
C2 C3 C9 C8 -6.50(18) . . . . ?
C2 C3 C9 C13 173.36(12) . . . . ?
C3 C4 C5 C6 -55.27(16) . . . . ?
C3 C4 C5 C14 126.14(12) . . . . ?
C3 C4 C25 C26 -153.37(10) . . . . ?
C3 C9 C13 C12 179.91(13) . . . . ?
C4 C3 C9 C8 171.36(11) . . . . ?
C4 C3 C9 C13 -8.77(18) . . . . ?
C4 C5 C6 N1 1.11(18) . . . . ?
C4 C5 C6 C17 178.26(12) . . . . ?
C4 C5 C14 C15 178.45(12) . . . . ?
C4 C25 C26 O5 29.98(17) . . . . ?
C4 C25 C26 C27 -149.88(11) . . . . ?
C5 C4 C25 C26 73.63(13) . . . . ?
C5 C6 C17 C16 3.8(2) . . . . ?
C5 C14 C15 C16 2.9(2) . . . . ?
C6 N1 C1 C2 -67.77(15) . . . . ?
C6 C5 C14 C15 -0.2(2) . . . . ?
C7 O1 C2 C1 -178.46(10) . . . . ?
C7 O1 C2 C3 1.24(18) . . . . ?
C7 C8 C9 C3 2.48(18) . . . . ?
C7 C8 C9 C13 -177.39(12) . . . . ?
C7 C8 C10 C11 177.46(12) . . . . ?
C8 C9 C13 C12 -0.2(2) . . . . ?
C8 C10 C11 C12 0.0(2) . . . . ?
C9 C3 C4 C5 -142.53(11) . . . . ?
C9 C3 C4 C25 86.96(13) . . . . ?
C9 C8 C10 C11 -1.9(2) . . . . ?
C10 C8 C9 C3 -178.18(11) . . . . ?
C10 C8 C9 C13 1.94(19) . . . . ?
C10 C11 C12 C13 1.7(2) . . . . ?
C11 C12 C13 C9 -1.6(2) . . . . ?
C14 C5 C6 N1 179.72(11) . . . . ?
C14 C5 C6 C17 -3.12(19) . . . . ?
C14 C15 C16 C17 -2.2(2) . . . . ?
C15 C16 C17 C6 -1.1(2) . . . . ?
C18 S1 N1 C1 69.42(10) . . . . ?
C18 S1 N1 C6 -102.62(11) . . . . ?
C18 C19 C20 C21 0.1(2) . . . . ?
C19 C18 C23 C22 2.29(19) . . . . ?
C19 C20 C21 C22 2.1(2) . . . . ?
C19 C20 C21 C24 -175.75(14) . . . . ?
C20 C21 C22 C23 -2.1(2) . . . . ?
C21 C22 C23 C18 0.0(2) . . . . ?
C23 C18 C19 C20 -2.3(2) . . . . ?
C24 C21 C22 C23 175.70(14) . . . . ?
C25 C4 C5 C6 76.35(15) . . . . ?
C25 C4 C5 C14 -102.24(13) . . . . ?
C25 C26 C27 C28 164.27(11) . . . . ?
C25 C26 C27 C32 -15.82(19) . . . . ?
C26 C27 C28 C29 -178.81(13) . . . . ?
C26 C27 C32 C31 179.96(15) . . . . ?
C27 C28 C29 C30 -1.0(2) . . . . ?
C28 C27 C32 C31 -0.1(2) . . . . ?
C28 C29 C30 C31 -0.4(3) . . . . ?
C29 C30 C31 C32 1.6(3) . . . . ?
C30 C31 C32 C27 -1.3(3) . . . . ?
C32 C27 C28 C29 1.3(2) . . . . ?
C2S O2S C3S C4S -93.3(5) . . . . ?
C3S O2S C2S O1S 3.9(5) . . . . ?
C3S O2S C2S C1S -176.6(4) . . . . ?
