#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:19:22 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286064 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/95/1569544.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_1569544
loop_
_publ_author_name
'Lu, Licheng'
'Lu, Ping'
_publ_section_title
;
 Enantioselective [3+2]-cycloaddition of 2,3-disubstituted cyclobutenones:
 vicinal quaternary stereocenters construction and skeletal
 functionalization.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              8355
_journal_page_last               8359
_journal_paper_doi               10.1039/d3sc02485g
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H31 N O8 S'
_chemical_formula_sum            'C30 H31 N O8 S'
_chemical_formula_weight         565.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2fz2k2
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-16 deposited with the CCDC.	2023-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.2370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.63180(10)
_cell_length_b                   7.14960(10)
_cell_length_c                   15.68420(10)
_cell_measurement_reflns_used    24674
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      74.2020
_cell_measurement_theta_min      3.5720
_cell_volume                     1389.32(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_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      7.00  87.00   1.00    1.00    --    0.00  77.00-120.00   80
  2  ω    -24.00  81.00   1.00    1.00    --    0.00  19.00  30.00  105
  3  ω     -6.00  19.00   1.00    1.00    --    0.00 -37.00 -90.00   25
  4  ω     45.00  72.00   1.00    1.00    --    0.00  37.00 120.00   27
  5  ω     40.00  78.00   1.00    1.00    --    0.00  57.00-150.00   38
  6  ω     59.00  84.00   1.00    1.00    --    0.00  37.00-180.00   25
  7  ω     31.00  57.00   1.00    1.00    --    0.00  37.00-180.00   26
  8  ω     29.00  60.00   1.00    1.00    --    0.00  57.00  30.00   31
  9  ω    -44.00  -9.00   1.00    1.00    --    0.00 -82.00-120.00   35
 10  ω    -19.00  26.00   1.00    1.00    --    0.00  37.00 120.00   45
 11  ω    -88.00 -48.00   1.00    1.00    --    0.00 -82.00-120.00   40
 12  ω    -56.00 -25.00   1.00    1.00    --    0.00 -37.00 -90.00   31
 13  ω    -21.00  13.00   1.00    1.00    --    0.00  57.00  30.00   34
 14  ω    -23.00  33.00   1.00    1.00    --    0.00  57.00-150.00   56
 15  ω     68.00  93.00   1.00    1.00    --   95.80  70.00  98.18   25
 16  ω    136.00 185.00   1.00    1.00    --   95.80  74.00 -87.31   49
 17  ω     71.00 185.00   1.00    1.00    --   95.80  61.00  63.85  114
 18  ω     66.00 123.00   1.00    1.00    --   95.80  74.00 -87.31   57
 19  ω      6.00 128.00   1.00    1.00    --   95.80 -82.00 131.81  122
 20  ω     71.00 180.00   1.00    1.00    --   95.80  63.00 129.34  109
 21  ω    109.00 167.00   1.00    1.00    --   95.80  63.00-137.48   58
 22  ω     72.00 120.00   1.00    1.00    --   95.80  61.00  90.00   48
 23  ω     48.00 117.00   1.00    1.00    --   95.80 -82.00-150.00   69
 24  ω     63.00 124.00   1.00    1.00    --   95.80  82.00 150.00   61
 25  ω     63.00 103.00   1.00    1.00    --   95.80  82.00-120.00   40
 26  ω     65.00  90.00   1.00    1.00    --   95.80  77.00 -30.00   25
 27  ω    112.00 138.00   1.00    1.00    --   95.80  77.00 -30.00   26
 28  ω     66.00  91.00   1.00    1.00    --   95.80  77.00 -60.00   25
 29  ω    100.00 126.00   1.00    1.00    --   95.80  77.00 -60.00   26
 30  ω     64.00  90.00   1.00    1.00    --   95.80  82.00   0.00   26
 31  ω     68.00  93.00   1.00    1.00    --   95.80  68.00-119.09   25
 32  ω      6.00 125.00   1.00    1.00    --   95.80 -82.00  30.00  119
 33  ω     65.00  91.00   1.00    1.00    --   95.80  77.00  30.00   26
 34  ω     70.00  96.00   1.00    1.00    --   95.80  63.00   3.64   26
 35  ω    142.00 167.00   1.00    1.00    --   95.80  54.00  23.89   25
 36  ω     65.00  90.00   1.00    1.00    --   95.80  77.00-150.00   25
 37  ω      6.00 120.00   1.00    1.00    --   95.80 -61.00 -90.00  114
 38  ω     63.00  88.00   1.00    1.00    --   95.80  82.00 120.00   25
 39  ω     65.00  90.00   1.00    1.00    --   95.80  77.00  60.00   25
 40  ω    115.00 142.00   1.00    1.00    --   95.80  81.00 137.48   27
 41  ω     66.00  91.00   1.00    1.00    --   95.80  77.00-180.00   25
 42  ω     62.00 121.00   1.00    1.00    --   95.80 -77.00  60.00   59
 43  ω     72.00  98.00   1.00    1.00    --   95.80  61.00 120.00   26
 44  ω     65.00  91.00   1.00    1.00    --   95.80  82.00 -90.00   26
 45  ω     71.00 185.00   1.00    1.00    --   95.80  61.00 -30.00  114
 46  ω     71.00  96.00   1.00    1.00    --   95.80  61.00-150.00   25
 47  ω     71.00 167.00   1.00    1.00    --   95.80  61.00-120.00   96
 48  ω     71.00 139.00   1.00    1.00    --   95.80  61.00   0.00   68
 49  ω     71.00 124.00   1.00    1.00    --   95.80  61.00  30.00   53
 50  ω     65.00  91.00   1.00    1.00    --   95.80  77.00-120.00   26
 51  ω     63.00  89.00   1.00    1.00    --   95.80  82.00 -60.00   26
 52  ω    123.00 180.00   1.00    1.00    --   95.80  82.00   0.00   57
 53  ω     58.00 124.00   1.00    1.00    --   95.80 -82.00 -60.00   66
 54  ω     75.00 100.00   1.00    1.00    --   95.80  45.00 -30.00   25
 55  ω     75.00 124.00   1.00    1.00    --   95.80  45.00 120.00   49
 56  ω    130.00 158.00   1.00    1.00    --   95.80  45.00 120.00   28
 57  ω     64.00  90.00   1.00    1.00    --   95.80  81.00 137.48   26
 58  ω     65.00  90.00   1.00    1.00    --   95.80  77.00 120.00   25
 59  ω     73.00  98.00   1.00    1.00    --   95.80  54.00  23.89   25
 60  ω     70.00 106.00   1.00    1.00    --   95.80  63.00-137.48   36
 61  ω     72.00 183.00   1.00    1.00    --   95.80  55.00-157.61  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1068932000
_diffrn_orient_matrix_UB_12      0.1067559000
_diffrn_orient_matrix_UB_13      0.0291519000
_diffrn_orient_matrix_UB_21      0.0089914000
_diffrn_orient_matrix_UB_22      -0.0778725000
_diffrn_orient_matrix_UB_23      0.0927124000
_diffrn_orient_matrix_UB_31      0.0628761000
_diffrn_orient_matrix_UB_32      -0.1702315000
_diffrn_orient_matrix_UB_33      -0.0241500000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29729
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details
;
 Flack x determined using 2223 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(6)
_refine_ls_extinction_coef       0.0060(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         4977
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0240
_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)+(0.0347P)²+0.2619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4926
_reflns_number_total             4977
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc02485g2.cif
_cod_data_source_block           exp_3074
_cod_depositor_comments
'Adding full bibliography for 1569539--1569545.cif.'
_cod_database_code               1569544
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_max   0.682
_shelx_estimated_absorpt_t_min   0.596
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C19(H19), C21(H21), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), 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 2.016
_oxdiff_exptl_absorpt_empirical_full_min 0.644
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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 -0.79042(4) -0.18187(6) -0.22563(3) 0.02382(13) Uani 1 1 d . . . . .
O1 O -0.69679(12) -0.0648(2) -0.20520(10) 0.0324(3) Uani 1 1 d . . . . .
O2 O -0.87758(13) -0.1304(2) -0.29471(10) 0.0339(4) Uani 1 1 d . . . . .
O3 O -0.92060(12) -0.6539(2) -0.27145(10) 0.0378(4) Uani 1 1 d . . . . .
O4 O -0.94486(11) -0.6257(2) -0.41625(9) 0.0319(3) Uani 1 1 d . . . . .
O5 O -0.78152(13) -0.5389(2) -0.53578(10) 0.0325(3) Uani 1 1 d . . . . .
O6 O -0.81479(13) -0.8452(2) -0.55349(9) 0.0318(3) Uani 1 1 d . . . . .
O7 O -0.55914(11) -0.5288(2) -0.43767(9) 0.0264(3) Uani 1 1 d . . . . .
O8 O -0.62720(13) -0.2721(2) -0.38571(10) 0.0318(4) Uani 1 1 d . . . . .
N1 N -0.75488(13) -0.3930(2) -0.24854(10) 0.0213(3) Uani 1 1 d . . . . .
C0AA C -0.72317(17) -0.6236(3) -0.08618(13) 0.0279(4) Uani 1 1 d . . . . .
H0AA H -0.779657 -0.674206 -0.128883 0.033 Uiso 1 1 calc R . . . .
C1 C -0.84018(16) -0.2086(3) -0.12909(13) 0.0249(4) Uani 1 1 d . . . . .
C2 C -0.77766(17) -0.1538(3) -0.05053(14) 0.0290(5) Uani 1 1 d . . . . .
H2 H -0.709597 -0.095679 -0.048615 0.035 Uiso 1 1 calc R . . . .
C3 C -0.81598(18) -0.1849(4) 0.02539(14) 0.0333(5) Uani 1 1 d . . . . .
H3 H -0.773027 -0.148775 0.079519 0.040 Uiso 1 1 calc R . . . .
C4 C -0.9156(2) -0.2677(3) 0.02396(15) 0.0334(5) Uani 1 1 d . . . . .
C5 C -0.97744(19) -0.3181(3) -0.05624(16) 0.0349(5) Uani 1 1 d . . . . .
H5 H -1.046577 -0.372444 -0.058527 0.042 Uiso 1 1 calc R . . . .
C6 C -0.94046(17) -0.2910(3) -0.13236(14) 0.0305(5) Uani 1 1 d . . . . .
H6 H -0.983081 -0.328115 -0.186469 0.037 Uiso 1 1 calc R . . . .
C7 C -0.9562(2) -0.3041(4) 0.10683(17) 0.0470(6) Uani 1 1 d . . . . .
H7A H -0.913379 -0.403948 0.139742 0.071 Uiso 1 1 calc GR . . . .
H7B H -1.032171 -0.342164 0.092601 0.071 Uiso 1 1 calc GR . . . .
H7C H -0.949534 -0.189756 0.141944 0.071 Uiso 1 1 calc GR . . . .
C8 C -0.64292(16) -0.5161(3) -0.11138(12) 0.0232(4) Uani 1 1 d . . . . .
C9 C -0.55898(18) -0.4485(3) -0.04802(14) 0.0323(5) Uani 1 1 d . . . . .
H9 H -0.502528 -0.378146 -0.064676 0.039 Uiso 1 1 calc R . . . .
C10 C -0.5571(2) -0.4831(4) 0.03948(15) 0.0401(6) Uani 1 1 d . . . . .
H10 H -0.499540 -0.436261 0.082368 0.048 Uiso 1 1 calc R . . . .
C11 C -0.6384(2) -0.5850(4) 0.06393(14) 0.0396(6) Uani 1 1 d . . . . .
H11 H -0.637982 -0.606063 0.123789 0.048 Uiso 1 1 calc R . . . .
C12 C -0.72089(19) -0.6569(3) 0.00128(14) 0.0352(5) Uani 1 1 d . . . . .
H12 H -0.776249 -0.729541 0.018297 0.042 Uiso 1 1 calc R . . . .
C13 C -0.51727(15) -0.6960(3) -0.26197(11) 0.0227(4) Uani 1 1 d . . . . .
C14 C -0.49778(17) -0.8813(3) -0.28163(13) 0.0272(4) Uani 1 1 d . . . . .
H14 H -0.554482 -0.970477 -0.287253 0.033 Uiso 1 1 calc R . . . .
C15 C -0.39581(19) -0.9368(4) -0.29309(15) 0.0368(5) Uani 1 1 d . . . . .
H15 H -0.384007 -1.063007 -0.307798 0.044 Uiso 1 1 calc R . . . .
C16 C -0.31215(19) -0.8110(4) -0.28334(16) 0.0431(6) Uani 1 1 d . . . . .
H16 H -0.243136 -0.848883 -0.292491 0.052 Uiso 1 1 calc R . . . .
C17 C -0.32951(18) -0.6286(4) -0.26005(16) 0.0420(6) Uani 1 1 d . . . . .
H17 H -0.271285 -0.542128 -0.251124 0.050 Uiso 1 1 calc R . . . .
C18 C -0.43108(17) -0.5705(3) -0.24957(14) 0.0327(5) Uani 1 1 d . . . . .
H18 H -0.441931 -0.444577 -0.233876 0.039 Uiso 1 1 calc R . . . .
C19 C -0.79428(15) -0.4712(3) -0.33529(12) 0.0214(4) Uani 1 1 d . . . . .
H19 H -0.814327 -0.367155 -0.378014 0.026 Uiso 1 1 calc R . . . .
C20 C -0.69572(15) -0.5783(3) -0.35622(12) 0.0200(4) Uani 1 1 d . . . . .
C21 C -0.63298(14) -0.6354(3) -0.26337(11) 0.0199(4) Uani 1 1 d . . . . .
H21 H -0.671771 -0.743951 -0.243389 0.024 Uiso 1 1 calc R . . . .
C22 C -0.64765(15) -0.4666(3) -0.20597(12) 0.0213(4) Uani 1 1 d . . . . .
H22 H -0.591058 -0.370998 -0.210033 0.026 Uiso 1 1 calc R . . . .
C23 C -0.89260(15) -0.5946(3) -0.33467(13) 0.0241(4) Uani 1 1 d . . . . .
C24 C -1.03289(19) -0.7601(4) -0.42740(17) 0.0416(6) Uani 1 1 d . . . . .
H24A H -1.057781 -0.785869 -0.489440 0.062 Uiso 1 1 calc GR . . . .
H24B H -1.092592 -0.708639 -0.403167 0.062 Uiso 1 1 calc GR . . . .
H24C H -1.007615 -0.876459 -0.397096 0.062 Uiso 1 1 calc GR . . . .
C25 C -0.72429(16) -0.7490(3) -0.41535(13) 0.0221(4) Uani 1 1 d . . . . .
H25A H -0.657757 -0.821129 -0.416763 0.027 Uiso 1 1 calc R . . . .
H25B H -0.774021 -0.830848 -0.390770 0.027 Uiso 1 1 calc R . . . .
C26 C -0.77648(15) -0.6954(3) -0.50668(12) 0.0240(4) Uani 1 1 d . . . . .
C27 C -0.8660(2) -0.8057(4) -0.64243(14) 0.0405(6) Uani 1 1 d . . . . .
H27A H -0.890004 -0.923072 -0.672347 0.061 Uiso 1 1 calc GR . . . .
H27B H -0.814309 -0.743527 -0.672174 0.061 Uiso 1 1 calc GR . . . .
H27C H -0.928370 -0.723885 -0.643038 0.061 Uiso 1 1 calc GR . . . .
C28 C -0.62630(15) -0.4389(3) -0.39562(12) 0.0223(4) Uani 1 1 d . . . . .
C29 C -0.4860(2) -0.4132(4) -0.47396(16) 0.0380(5) Uani 1 1 d . . . . .
H29A H -0.526879 -0.336970 -0.521053 0.057 Uiso 1 1 calc GR . . . .
H29B H -0.434827 -0.492552 -0.496928 0.057 Uiso 1 1 calc GR . . . .
H29C H -0.446428 -0.331163 -0.428644 0.057 Uiso 1 1 calc GR . . . .
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'
N N 0.0311 0.0180 '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
O1 S1 O2 119.85(10) . . ?
O1 S1 N1 109.77(9) . . ?
O1 S1 C1 106.79(10) . . ?
O2 S1 N1 105.90(9) . . ?
O2 S1 C1 109.13(9) . . ?
N1 S1 C1 104.37(9) . . ?
C23 O4 C24 116.59(18) . . ?
C26 O6 C27 114.83(18) . . ?
C28 O7 C29 115.93(17) . . ?
C19 N1 S1 119.88(13) . . ?
C19 N1 C22 113.41(15) . . ?
C22 N1 S1 119.59(13) . . ?
C8 C0AA H0AA 120.0 . . ?
C12 C0AA H0AA 120.0 . . ?
C12 C0AA C8 120.0(2) . . ?
C2 C1 S1 119.84(15) . . ?
C2 C1 C6 120.73(18) . . ?
C6 C1 S1 119.38(16) . . ?
C1 C2 H2 120.5 . . ?
C1 C2 C3 118.96(19) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 C5 118.2(2) . . ?
C3 C4 C7 121.3(2) . . ?
C5 C4 C7 120.5(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.4(2) . . ?
C6 C5 H5 119.3 . . ?
C1 C6 H6 120.4 . . ?
C5 C6 C1 119.2(2) . . ?
C5 C6 H6 120.4 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C0AA C8 C9 119.07(19) . . ?
C0AA C8 C22 121.07(17) . . ?
C9 C8 C22 119.83(19) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.5(2) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0(2) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0(2) . . ?
C12 C11 H11 120.0 . . ?
C0AA C12 H12 119.8 . . ?
C11 C12 C0AA 120.4(2) . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C18 118.42(19) . . ?
C14 C13 C21 118.58(18) . . ?
C18 C13 C21 122.7(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.5(2) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.7(2) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.4 . . ?
C15 C16 C17 119.3(2) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.7(2) . . ?
C18 C17 H17 119.6 . . ?
C13 C18 H18 119.8 . . ?
C17 C18 C13 120.3(2) . . ?
C17 C18 H18 119.8 . . ?
N1 C19 H19 109.5 . . ?
N1 C19 C20 104.10(15) . . ?
N1 C19 C23 110.14(15) . . ?
C20 C19 H19 109.5 . . ?
C23 C19 H19 109.5 . . ?
C23 C19 C20 113.83(16) . . ?
C19 C20 C21 102.31(14) . . ?
C25 C20 C19 114.67(15) . . ?
C25 C20 C21 111.74(15) . . ?
C25 C20 C28 111.05(15) . . ?
C28 C20 C19 108.06(15) . . ?
C28 C20 C21 108.53(14) . . ?
C13 C21 C20 113.42(14) . . ?
C13 C21 H21 107.6 . . ?
C13 C21 C22 116.10(16) . . ?
C20 C21 H21 107.6 . . ?
C22 C21 C20 103.99(14) . . ?
C22 C21 H21 107.6 . . ?
N1 C22 C8 112.43(16) . . ?
N1 C22 C21 102.60(14) . . ?
N1 C22 H22 109.3 . . ?
C8 C22 C21 113.78(16) . . ?
C8 C22 H22 109.3 . . ?
C21 C22 H22 109.3 . . ?
O3 C23 O4 124.35(19) . . ?
O3 C23 C19 125.75(18) . . ?
O4 C23 C19 109.89(16) . . ?
O4 C24 H24A 109.5 . . ?
O4 C24 H24B 109.5 . . ?
O4 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.1 . . ?
C20 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 C20 112.38(17) . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
O5 C26 O6 123.36(18) . . ?
O5 C26 C25 125.30(18) . . ?
O6 C26 C25 111.32(18) . . ?
O6 C27 H27A 109.5 . . ?
O6 C27 H27B 109.5 . . ?
O6 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O7 C28 C20 110.71(16) . . ?
O8 C28 O7 124.32(19) . . ?
O8 C28 C20 124.82(18) . . ?
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 . . ?
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 O1 1.4331(15) . ?
S1 O2 1.4340(16) . ?
S1 N1 1.6347(17) . ?
S1 C1 1.759(2) . ?
O3 C23 1.194(3) . ?
O4 C23 1.339(2) . ?
O4 C24 1.454(3) . ?
O5 C26 1.205(3) . ?
O6 C26 1.335(3) . ?
O6 C27 1.447(3) . ?
O7 C28 1.337(2) . ?
O7 C29 1.437(3) . ?
O8 C28 1.203(3) . ?
N1 C19 1.465(2) . ?
N1 C22 1.485(2) . ?
C0AA H0AA 0.9500 . ?
C0AA C8 1.389(3) . ?
C0AA C12 1.387(3) . ?
C1 C2 1.384(3) . ?
C1 C6 1.389(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(3) . ?
C4 C5 1.393(3) . ?
C4 C7 1.510(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.378(3) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.391(3) . ?
C8 C22 1.515(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.373(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(3) . ?
C13 C18 1.395(3) . ?
C13 C21 1.520(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.393(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.373(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(3) . ?
C18 H18 0.9500 . ?
C19 H19 1.0000 . ?
C19 C20 1.550(3) . ?
C19 C23 1.525(3) . ?
C20 C21 1.570(2) . ?
C20 C25 1.533(3) . ?
C20 C28 1.535(3) . ?
C21 H21 1.0000 . ?
C21 C22 1.539(3) . ?
C22 H22 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.505(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
