#------------------------------------------------------------------------------
#$Date: 2025-03-21 01:42:24 +0200 (Fri, 21 Mar 2025) $
#$Revision: 298546 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/01/7250156.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_7250156
loop_
_publ_author_name
'Winson, Cinu'
'Kandasamy, Saravanan'
'Divya, Indira S.'
'Wozniak, Krzysztof'
'Varughese, Sunil'
_publ_section_title
;
 Polymorphs and stoichiometric variants of crown ether-based molecular
 complexes. Exploring the landscape of conformational flexibility and
 supramolecular interactions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00025D
_journal_year                    2025
_chemical_formula_moiety         'C2 H4 N2 S2, C20 H36 O6'
_chemical_formula_sum            'C22 H40 N2 O6 S2'
_chemical_formula_weight         492.705
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-03-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-23 deposited with the CCDC.	2025-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                91.7000(19)
_cell_angle_beta                 105.5010(19)
_cell_angle_gamma                101.171(2)
_cell_formula_units_Z            3
_cell_length_a                   10.1460(2)
_cell_length_b                   14.1440(4)
_cell_length_c                   14.5050(3)
_cell_measurement_reflns_used    16103
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.3830
_cell_measurement_theta_min      3.2020
_cell_volume                     1960.51(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9855
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -42.00   0.50    0.05    --    0.00 140.00  -7.00   64
  2  ω    -70.00 -19.00   0.50    0.05    --    0.00 130.00 178.00  102
  3  ω    -50.00 -10.00   0.50    0.05    --    0.00 -77.00 -60.00   80
  4  ω     15.00  42.00   0.50    0.05    --    0.00  57.00 -60.00   54
  5  ω    -93.00 -42.00   0.50    0.05    --    0.00-178.00   0.00  102
  6  ω    -34.00  -9.00   0.50    0.05    --    0.00 -77.00-120.00   50
  7  ω    -85.00 -58.00   0.50    0.05    --    0.00 -77.00 -60.00   54
  8  ω    -86.00 -55.00   0.50    0.05    --    0.00 -77.00  60.00   62
  9  ω     54.00  80.00   0.50    0.05    --    0.00  57.00 -60.00   52
 10  ω    -52.00  -8.00   0.50    0.05    --    0.00 -77.00  60.00   88
 11  ω    -74.00 -38.00   0.50    0.05    --    0.00 -77.00-120.00   72
 12  ω    -35.00  -2.00   0.50    0.05    --    0.00  57.00 -60.00   66
 13  ω    -33.00   4.00   0.50    0.05    --   18.00 103.00  42.89   74
 14  ω    -49.00 -24.00   0.50    0.05    --   30.00 146.00  40.30   50
 15  ω     -1.00  24.00   0.50    0.08    --   50.00  95.00-107.50   50
 16  ω      2.00  27.00   0.50    0.08    --   54.00  96.00 107.67   50
 17  ω      8.00  34.00   0.50    0.08    --   58.00  93.00  18.19   52
 18  ω      8.00  34.00   0.50    0.08    --   58.00  93.00 -69.03   52
 19  ω     15.00  40.00   0.50    0.08    --   62.00  89.00 154.19   50
 20  ω     14.00  41.00   0.50    0.08    --   62.00  91.00 109.17   54
 21  ω     17.00  42.00   0.50    0.08    --   66.00  90.00 -86.96   50
 22  ω     17.00  42.00   0.50    0.08    --   66.00  90.00-112.05   50
 23  ω     17.00  42.00   0.50    0.08    --   66.00  90.00 -12.21   50
 24  ω     16.00  41.00   0.50    0.08    --   66.00  92.00  94.70   50
 25  ω     16.00  42.00   0.50    0.08    --   66.00  92.00-172.49   52
 26  ω     17.00  42.00   0.50    0.08    --   66.00  90.00  36.14   50
 27  ω     29.00 103.00   0.50    0.08    --   66.57 -77.00  90.00  148
 28  ω     -8.00 102.00   0.50    0.08    --   66.57 -61.00-180.00  220
 29  ω     52.00  79.00   0.50    0.08    --   66.57 -94.00   0.00   54
 30  ω    -22.00 135.00   0.50    0.08    --   66.57 -30.00 -30.00  314
 31  ω     -2.00  81.00   0.50    0.08    --   66.57 -61.00-120.00  166
 32  ω     53.00  98.00   0.50    0.08    --   66.57 -94.00 120.00   90
 33  ω     36.00 109.00   0.50    0.08    --   66.57 -77.00 -30.00  146
 34  ω     70.00 106.00   0.50    0.08    --   70.00  75.00 176.54   72
 35  ω     41.00 109.00   0.50    0.08    --   70.00  76.00   5.86  136
 36  ω     29.00  63.00   0.50    0.08    --   70.00  75.00 176.54   68
 37  ω     80.00 108.00   0.50    0.08    --   74.00  77.00  50.56   56
 38  ω     31.00  57.00   0.50    0.08    --   74.00  77.00  50.56   52
 39  ω     75.00 101.00   0.50    0.08    --   74.00  75.00 -30.27   52
 40  ω     36.00  63.00   0.50    0.08    --   74.00  75.00 -30.27   54
 41  ω     35.00  61.00   0.50    0.08    --   78.00  77.00 -92.80   52
 42  ω     36.00  62.00   0.50    0.08    --   78.00  77.00 123.64   52
 43  ω     76.00 109.00   0.50    0.08    --   78.00  77.00  79.76   66
 44  ω     35.00  66.00   0.50    0.08    --   78.00  77.00  79.76   62
 45  ω     84.00 109.00   0.50    0.08    --   78.00  77.00 -92.80   50
 46  ω     68.00 109.00   0.50    0.08    --   78.00  77.00 123.64   82
 47  ω     36.00  62.00   0.50    0.08    --   78.00  75.00 -62.83   52
 48  ω     40.00  66.00   0.50    0.08    --   82.00  75.00 138.57   52
 49  ω     84.00 109.00   0.50    0.08    --   82.00  76.00 -17.81   50
 50  ω     41.00  67.00   0.50    0.08    --   82.00  76.00 -17.81   52
 51  ω     83.00 109.00   0.50    0.08    --   82.00  75.00 138.57   52
 52  ω     40.00  70.00   0.50    0.08    --   82.00  76.00-117.42   60
 53  ω     44.00  70.00   0.50    0.08    --   86.00  77.00 159.68   52
 54  ω     45.00  71.00   0.50    0.08    --   86.00  74.00  22.03   52
 55  ω     69.00  95.00   0.50    0.08    --   86.00  77.00-148.18   52
 56  ω     43.00  68.00   0.50    0.08    --   86.00  77.00-148.18   50
 57  ω     84.00 109.00   0.50    0.08    --   86.00  77.00 -85.61   50
 58  ω     43.00  69.00   0.50    0.08    --   86.00  77.00 -85.61   52
 59  ω     49.00  75.00   0.50    0.08    --   90.00  76.00 172.82   52
 60  ω     80.00 109.00   0.50    0.08    --   90.00  77.00  63.86   58
 61  ω     47.00  72.00   0.50    0.08    --   90.00  77.00  63.86   50
 62  ω     48.00  75.00   0.50    0.08    --   90.00  76.00 -61.74   54
 63  ω     62.00  88.00   0.50    0.08    --   94.00  66.00-162.42   52
 64  ω    120.00 146.00   0.50    0.08    --   94.00  72.00  68.60   52
 65  ω     53.00  79.00   0.50    0.08    --   94.00  72.00  68.60   52
 66  ω     53.00  89.00   0.50    0.08    --   94.00  73.00-114.11   72
 67  ω    121.00 169.00   0.50    0.08    --   94.00  66.00-162.42   96
 68  ω     89.00 135.00   0.50    0.08    --   94.00  70.00 111.52   92
 69  ω     55.00  81.00   0.50    0.08    --   94.00  70.00 111.52   52
 70  ω     51.00  77.00   0.50    0.08    --   94.00  77.00  84.67   52
 71  ω     52.00  78.00   0.50    0.08    --   94.00  76.00 -12.05   52
 72  ω    138.00 175.00   0.50    0.08    --   94.00  70.00 111.52   74
 73  ω     56.00  81.00   0.50    0.08    --   98.00  75.00 149.12   50
 74  ω     56.00  81.00   0.50    0.08    --   98.00  77.00 -31.01   50
 75  ω     56.00  92.00   0.50    0.08    --   98.00  76.00 116.07   72
 76  ω     55.00 109.00   0.50    0.08    --   98.00  77.00  21.32  108
 77  ω    107.00 167.00   0.50    0.08    --   98.00  68.00 -79.05  120
 78  ω     61.00  87.00   0.50    0.08    --   98.00  68.00 -79.05   52
 79  ω     66.00 108.00   0.50    0.08    --  102.00  63.00-148.64   84
 80  ω     60.00  85.00   0.50    0.08    --  102.00  76.00 -72.22   50
 81  ω     64.00  89.00   0.50    0.08    --  106.00  75.00 154.93   50
 82  ω     64.00  89.00   0.50    0.08    --  106.00  76.00 -35.45   50
 83  ω    153.00 178.00   0.50    0.08    --  110.00  73.00-111.86   50
 84  ω     69.00  98.00   0.50    0.08    --  110.00  73.00-111.86   58
 85  ω    139.00 176.00   0.50    0.08    --  110.00  69.00 -20.70   74
 86  ω     73.00  99.00   0.50    0.08    --  110.00  69.00 -20.70   52
 87  ω     68.00 109.00   0.50    0.08    --  110.00  76.00  87.21   82
 88  ω    153.00 178.00   0.50    0.08    --  114.00  72.00 137.65   50
 89  ω     73.00 113.00   0.50    0.08    --  114.00  72.00 137.65   80
 90  ω    133.00 176.00   0.50    0.08    --  114.00  64.00 -57.58   86
 91  ω     79.00 118.00   0.50    0.08    --  114.00  64.00 -57.58   78
 92  ω    146.00 178.00   0.50    0.08    --  114.00  73.00   1.82   64
 93  ω    109.00 139.00   0.50    0.08    --  114.00  73.00   1.82   60
 94  ω     74.00 104.00   0.50    0.08    --  114.00  73.00   1.82   60
 95  ω    129.00 155.00   0.50    0.08    --  114.00  72.00-147.62   52
 96  ω     73.00 107.00   0.50    0.08    --  114.00  72.00-147.62   68
 97  ω    126.00 171.00   0.50    0.08    --  114.00  68.00  64.84   90
 98  ω     75.00 105.00   0.50    0.08    --  114.00  68.00  64.84   60
 99  ω     91.00 153.00   0.50    0.08    --  121.75  50.00  60.00  124
100  ω    121.00 178.00   0.50    0.08    --  121.75  63.00  90.00  114
101  ω     78.00 137.00   0.50    0.08    --  121.75  45.00 -92.50  118
102  ω     83.00 166.00   0.50    0.08    --  121.75  50.00-120.00  166
103  ω     62.00 106.00   0.50    0.08    --  121.75 -96.00  77.06   88
104  ω    125.00 151.00   0.50    0.08    --  121.75 -37.00-150.00   52
105  ω     85.00 152.00   0.50    0.08    --  121.75  63.00 120.00  134
106  ω     85.00 113.00   0.50    0.08    --  121.75  63.00  90.00   56
107  ω     46.00 103.00   0.50    0.08    --  121.75 -91.00 -90.00  114
108  ω     72.00 114.00   0.50    0.08    --  121.75 -37.00-150.00   84
109  ω     35.00  66.00   0.50    0.08    --  121.75 -37.00-150.00   62
110  ω     83.00 174.00   0.50    0.08    --  121.75  68.00 139.36  182
111  ω     81.00 107.00   0.50    0.08    --  121.75  77.00 156.97   52
112  ω     84.00 112.00   0.50    0.08    --  121.75-126.00 175.41   56
113  ω     89.00 177.00   0.50    0.08    --  121.75  63.00-180.00  176
114  ω     95.00 120.00   0.50    0.08    --  121.75-135.00  59.47   50
115  ω    127.00 170.00   0.50    0.08    --  121.75  68.00-169.49   86
116  ω     83.00 116.00   0.50    0.08    --  121.75  68.00-169.49   66
117  ω    126.00 178.00   0.50    0.08    --  121.75  48.00 -13.46  104
118  ω    124.00 168.00   0.50    0.08    --  121.75  63.00  30.00   88
119  ω     70.00 161.00   0.50    0.08    --  121.75 -50.00  30.00  182
120  ω     62.00 108.00   0.50    0.08    --  121.75-106.00 160.75   92
121  ω     46.00 103.00   0.50    0.08    --  121.75 -91.00 -60.00  114
122  ω     92.00 119.00   0.50    0.08    --  121.75  48.00 -13.46   54
123  ω     88.00 143.00   0.50    0.08    --  121.75  63.00 -90.00  110
124  ω    131.00 162.00   0.50    0.08    --  121.75 -77.00-150.00   62
125  ω     54.00 118.00   0.50    0.08    --  121.75 -77.00-150.00  128
126  ω    123.00 161.00   0.50    0.08    --  121.75 -12.00-150.00   76
127  ω     86.00 112.00   0.50    0.08    --  121.75  63.00  30.00   52
128  ω     30.00  82.00   0.50    0.08    --  121.75 -12.00-150.00  104
129  ω     51.00 105.00   0.50    0.08    --  121.75 -91.00  30.00  108
130  ω     56.00 106.00   0.50    0.08    --  121.75 -98.00-161.13  100
131  ω     53.00  79.00   0.50    0.08    --  121.75 -91.00-180.00   52
132  ω     80.00 106.00   0.50    0.08    --  121.75 -91.00-150.00   52
133  ω     85.00 151.00   0.50    0.08    --  121.75  50.00 -30.00  132
134  ω     47.00  78.00   0.50    0.08    --  121.75 -91.00 120.00   62
135  ω     87.00 162.00   0.50    0.08    --  121.75  50.00 120.00  150
136  ω     46.00  75.00   0.50    0.08    --  121.75 -91.00-150.00   58
137  ω     80.00 107.00   0.50    0.08    --  121.75  77.00 -88.42   54
138  ω     82.00 177.00   0.50    0.08    --  121.75  48.00  12.71  190
139  ω     38.00 174.00   0.50    0.08    --  121.75 -37.00 -30.00  272
140  ω     49.00 106.00   0.50    0.08    --  121.75 -91.00   0.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1164058000
_diffrn_orient_matrix_UB_12      -0.0534387000
_diffrn_orient_matrix_UB_13      -0.0875100000
_diffrn_orient_matrix_UB_21      -0.0816778000
_diffrn_orient_matrix_UB_22      -0.0486126000
_diffrn_orient_matrix_UB_23      0.0675653000
_diffrn_orient_matrix_UB_31      -0.0757969000
_diffrn_orient_matrix_UB_32      0.0848519000
_diffrn_orient_matrix_UB_33      -0.0038870000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9855
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47546
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9855
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.69
_diffrn_reflns_theta_min         4.31
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.160
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       block
_exptl_crystal_F_000             802.474
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.4346
_refine_diff_density_min         -0.3622
_refine_diff_density_rms         0.0491
_refine_ls_d_res_high            0.7891
_refine_ls_d_res_low             10.2629
_refine_ls_goodness_of_fit_ref   1.0253
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    86
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8228
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.0237
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          -0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0665P)²+0.4219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7384
_reflns_number_total             8228
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5ce00025d2.cif
_cod_data_source_block           exp_89_red1_abs1
_cod_database_code               7250156
_chemical_oxdiff_formula         'C32 H48 S2 N2 F9 I1'
_chemical_oxdiff_usercomment     '100K '
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H21a-N21
 0.89 with sigma of 0.04
 H21b-N21
 0.89 with sigma of 0.04
 S11-C11 \\sim S11-C11A
 with sigma of 0.02
 S12-C12 \\sim S12-C12A
 with sigma of 0.02
 N11-C11 \\sim N11-C11A
 with sigma of 0.02
 N11-C12 \\sim N11-C12A
 with sigma of 0.04
 N12-C12 \\sim N12-C12A
 with sigma of 0.02
 S11-C12 \\sim S11-C12A
 with sigma of 0.04
 C11-C12 \\sim C11A-C12A
 with sigma of 0.02
 S12-C11 \\sim S12-C11A
 with sigma of 0.04
 N12-C11 \\sim N12-C11A
 with sigma of 0.04
 S21-C21A \\sim S21-C21
 with sigma of 0.02
 N21-C21A \\sim N21-C21
 with sigma of 0.02
3. Others
 Sof(C11A)=Sof(C12A)=1-FVAR(1)
 Sof(C11)=Sof(C12)=FVAR(1)
 Sof(C21)=1-FVAR(2)
 Sof(C21A)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C33(H33), C38(H38), C51(H51), C56(H56), C61(H61), C66(H66)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31a,H31b), C32(H32a,H32b), C34(H34a,H34b), C35(H35a,H35b), C36(H36a,
 H36b), C37(H37a,H37b), C39(H39a,H39b), C40(H40a,H40b), C52(H52a,H52b),
 C53(H53a,H53b), C54(H54a,H54b), C55(H55a,H55b), C57(H57a,H57b), C58(H58a,H58b),
  C62(H62a,H62b), C63(H63a,H63b), C64(H64a,H64b), C65(H65a,H65b), C67(H67a,
 H67b), C68(H68a,H68b), C69(H69a,H69b), C70(H70a,H70b), C59(H59a,H59b),
 C60(H60a,H60b)
;
_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 1.321
_oxdiff_exptl_absorpt_empirical_full_min 0.805
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -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_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
S11 S 0.79263(5) 0.30078(4) 0.54229(3) 0.05426(13) Uani 1.000000 D . .
S12 S 0.50884(5) 0.29740(4) 0.71902(4) 0.05731(14) Uani 1.000000 D . .
N11 N 0.6064(2) 0.40781(10) 0.58857(12) 0.0469(3) Uani 1.000000 D . .
H11a H 0.555(3) 0.438(2) 0.6075(19) 0.076(8) Uiso 1.000000 . . .
H11b H 0.644(3) 0.4268(18) 0.5552(19) 0.061(7) Uiso 1.000000 . . .
N12 N 0.7085(2) 0.19844(11) 0.68270(13) 0.0511(4) Uani 1.000000 D . .
H12a H 0.762(3) 0.168(2) 0.668(2) 0.079(8) Uiso 1.000000 . . .
H12b H 0.674(3) 0.1800(19) 0.719(2) 0.068(8) Uiso 1.000000 . . .
C11 C 0.6752(4) 0.3327(2) 0.5975(2) 0.0345(9) Uiso 0.419(4) D P 1
C12 C 0.6308(4) 0.2692(2) 0.6702(2) 0.0345(9) Uiso 0.419(4) D P 1
C11A C 0.6030(3) 0.33063(18) 0.64018(18) 0.0350(7) Uiso 0.581(4) D P 2
C12A C 0.7055(2) 0.27126(17) 0.62436(17) 0.0332(6) Uiso 0.581(4) D P 2
S21 S 0.99773(5) -0.11233(3) 0.89418(3) 0.04360(11) Uani 1.000000 D . .
C21 C 1.0042(6) -0.0525(4) 0.9999(4) 0.033(2) Uiso 0.227(6) D P 2
H21a H 0.9804(18) 0.1218(12) 0.9324(12) 0.029(4) Uiso 1.000000 D . .
O31 O 0.65548(10) 0.59605(7) 0.70012(7) 0.0340(2) Uani 1.000000 . . .
O32 O 0.37328(10) 0.51667(7) 0.60569(7) 0.0339(2) Uani 1.000000 . . .
O33 O 0.19780(10) 0.39919(7) 0.44131(7) 0.0331(2) Uani 1.000000 . . .
C31 C 1.04545(16) 0.63449(13) 0.78498(12) 0.0448(3) Uani 1.000000 . . .
H31a H 1.06388(16) 0.68834(13) 0.83496(12) 0.0537(4) Uiso 1.000000 R . .
H31b H 1.10675(16) 0.58925(13) 0.81075(12) 0.0537(4) Uiso 1.000000 R . .
C32 C 0.89207(16) 0.58154(11) 0.76220(11) 0.0391(3) Uani 1.000000 . . .
H32a H 0.87585(16) 0.52324(11) 0.71786(11) 0.0469(4) Uiso 1.000000 R . .
H32b H 0.87079(16) 0.56051(11) 0.82207(11) 0.0469(4) Uiso 1.000000 R . .
C33 C 0.79618(14) 0.64768(10) 0.71641(10) 0.0335(3) Uani 1.000000 . . .
H33 H 0.81217(14) 0.70504(10) 0.76305(10) 0.0402(3) Uiso 1.000000 R . .
C34 C 0.55496(15) 0.65427(10) 0.67278(11) 0.0359(3) Uani 1.000000 . . .
H34a H 0.55024(15) 0.67374(10) 0.60717(11) 0.0431(3) Uiso 1.000000 R . .
H34b H 0.58187(15) 0.71355(10) 0.71734(11) 0.0431(3) Uiso 1.000000 R . .
C35 C 0.41493(15) 0.59745(11) 0.67548(11) 0.0377(3) Uani 1.000000 . . .
H35a H 0.34497(15) 0.63890(11) 0.66159(11) 0.0452(4) Uiso 1.000000 R . .
H35b H 0.42101(15) 0.57490(11) 0.74016(11) 0.0452(4) Uiso 1.000000 R . .
C36 C 0.23574(15) 0.46501(11) 0.60091(11) 0.0381(3) Uani 1.000000 . . .
H36a H 0.23038(15) 0.44897(11) 0.66596(11) 0.0457(4) Uiso 1.000000 R . .
H36b H 0.16716(15) 0.50574(11) 0.57599(11) 0.0457(4) Uiso 1.000000 R . .
C37 C 0.20150(16) 0.37382(11) 0.53596(10) 0.0371(3) Uani 1.000000 . . .
H37a H 0.10962(16) 0.33478(11) 0.53667(10) 0.0445(4) Uiso 1.000000 R . .
H37b H 0.27331(16) 0.33484(11) 0.55836(10) 0.0445(4) Uiso 1.000000 R . .
C38 C 0.17103(14) 0.31642(10) 0.37501(10) 0.0330(3) Uani 1.000000 . . .
H38 H 0.23417(14) 0.27209(10) 0.40298(10) 0.0396(3) Uiso 1.000000 R . .
C39 C 0.01891(15) 0.26133(11) 0.35000(11) 0.0390(3) Uani 1.000000 . . .
H39a H 0.00588(15) 0.20400(11) 0.30510(11) 0.0468(4) Uiso 1.000000 R . .
H39b H -0.00317(15) 0.23844(11) 0.40907(11) 0.0468(4) Uiso 1.000000 R . .
C40 C -0.08033(15) 0.32558(12) 0.30406(12) 0.0431(3) Uani 1.000000 . . .
H40a H -0.07328(15) 0.37987(12) 0.35100(12) 0.0517(4) Uiso 1.000000 R . .
H40b H -0.17773(15) 0.28772(12) 0.28606(12) 0.0517(4) Uiso 1.000000 R . .
O51 O 1.17658(11) 0.19890(7) 0.81387(7) 0.0380(2) Uani 1.000000 . . .
O52 O 1.06657(10) 0.31615(7) 0.92147(7) 0.0373(2) Uani 1.000000 . . .
O53 O 0.79126(11) 0.22042(8) 0.90368(7) 0.0385(2) Uani 1.000000 . . .
O54 O 0.59417(11) 0.05235(7) 0.81234(7) 0.0379(2) Uani 1.000000 . . .
O55 O 0.65541(10) -0.00804(7) 0.64412(7) 0.0355(2) Uani 1.000000 . . .
O56 O 0.94231(10) 0.08001(7) 0.68156(7) 0.0361(2) Uani 1.000000 . . .
C51 C 1.26347(15) 0.27853(11) 0.87829(10) 0.0381(3) Uani 1.000000 . . .
H51 H 1.34255(15) 0.30659(11) 0.85176(10) 0.0458(4) Uiso 1.000000 R . .
C52 C 1.32413(16) 0.23895(12) 0.97339(11) 0.0419(3) Uani 1.000000 . . .
H52a H 1.24729(16) 0.20843(12) 0.99981(11) 0.0503(4) Uiso 1.000000 R . .
H52b H 1.37579(16) 0.18890(12) 0.96275(11) 0.0503(4) Uiso 1.000000 R . .
C53 C 1.42313(17) 0.32060(14) 1.04529(12) 0.0482(4) Uani 1.000000 . . .
H53a H 1.45945(17) 0.29447(14) 1.10744(12) 0.0578(4) Uiso 1.000000 R . .
H53b H 1.50363(17) 0.34795(14) 1.02101(12) 0.0578(4) Uiso 1.000000 R . .
C54 C 1.34663(18) 0.39985(13) 1.06000(12) 0.0491(4) Uani 1.000000 . . .
H54a H 1.27136(18) 0.37369(13) 1.08962(12) 0.0589(5) Uiso 1.000000 R . .
H54b H 1.41277(18) 0.45326(13) 1.10445(12) 0.0589(5) Uiso 1.000000 R . .
C55 C 1.28335(18) 0.43896(12) 0.96469(12) 0.0455(4) Uani 1.000000 . . .
H55a H 1.35955(18) 0.47143(12) 0.93866(12) 0.0546(4) Uiso 1.000000 R . .
H55b H 1.22999(18) 0.48769(12) 0.97599(12) 0.0546(4) Uiso 1.000000 R . .
C56 C 1.18642(15) 0.35842(11) 0.89114(11) 0.0378(3) Uani 1.000000 . . .
H56 H 1.15480(15) 0.38582(11) 0.82817(11) 0.0454(4) Uiso 1.000000 R . .
C57 C 0.95237(16) 0.36223(11) 0.88860(11) 0.0407(3) Uani 1.000000 . . .
H57a H 0.91756(16) 0.35222(11) 0.81770(11) 0.0488(4) Uiso 1.000000 R . .
H57b H 0.98324(16) 0.43265(11) 0.90700(11) 0.0488(4) Uiso 1.000000 R . .
C58 C 0.83736(16) 0.32089(12) 0.93211(12) 0.0425(3) Uani 1.000000 . . .
H58a H 0.87198(16) 0.33129(12) 1.00299(12) 0.0510(4) Uiso 1.000000 R . .
H58b H 0.75836(16) 0.35401(12) 0.91054(12) 0.0510(4) Uiso 1.000000 R . .
C59 C 0.67635(17) 0.17973(13) 0.93826(12) 0.0446(3) Uani 1.000000 . . .
C60 C 0.63749(17) 0.07230(12) 0.91378(11) 0.0434(3) Uani 1.000000 . . .
C61 C 0.56416(16) -0.04877(11) 0.78214(11) 0.0396(3) Uani 1.000000 . . .
H61 H 0.64639(16) -0.07731(11) 0.81283(11) 0.0475(4) Uiso 1.000000 R . .
C62 C 0.43370(18) -0.10381(12) 0.80652(13) 0.0474(4) Uani 1.000000 . . .
H62a H 0.41749(18) -0.17328(12) 0.78525(13) 0.0569(4) Uiso 1.000000 R . .
H62b H 0.44883(18) -0.09779(12) 0.87694(13) 0.0569(4) Uiso 1.000000 R . .
C63 C 0.30532(17) -0.06393(13) 0.75746(13) 0.0479(4) Uani 1.000000 . . .
H63a H 0.22184(17) -0.10153(13) 0.77259(13) 0.0575(4) Uiso 1.000000 R . .
H63b H 0.31868(17) 0.00427(13) 0.78216(13) 0.0575(4) Uiso 1.000000 R . .
C64 C 0.28203(16) -0.06985(12) 0.64926(12) 0.0454(4) Uani 1.000000 . . .
H64a H 0.25966(16) -0.13858(12) 0.62394(12) 0.0544(4) Uiso 1.000000 R . .
H64b H 0.20123(16) -0.04092(12) 0.61907(12) 0.0544(4) Uiso 1.000000 R . .
C65 C 0.41135(15) -0.01690(11) 0.62258(11) 0.0395(3) Uani 1.000000 . . .
H65a H 0.39548(15) -0.02534(11) 0.55219(11) 0.0474(4) Uiso 1.000000 R . .
H65b H 0.42854(15) 0.05313(11) 0.64183(11) 0.0474(4) Uiso 1.000000 R . .
C66 C 0.53777(15) -0.05698(10) 0.67303(11) 0.0367(3) Uani 1.000000 . . .
H66 H 0.51912(15) -0.12707(10) 0.65057(11) 0.0440(4) Uiso 1.000000 R . .
C67 C 0.76100(16) -0.06189(11) 0.65220(13) 0.0441(3) Uani 1.000000 . . .
H67a H 0.79686(16) -0.07548(11) 0.71987(13) 0.0529(4) Uiso 1.000000 R . .
H67b H 0.72209(16) -0.12439(11) 0.61265(13) 0.0529(4) Uiso 1.000000 R . .
C68 C 0.87739(16) -0.00509(11) 0.61869(12) 0.0426(3) Uani 1.000000 . . .
H68a H 0.84001(16) 0.01270(11) 0.55272(12) 0.0511(4) Uiso 1.000000 R . .
H68b H 0.94716(16) -0.04496(11) 0.61749(12) 0.0511(4) Uiso 1.000000 R . .
C69 C 1.05871(16) 0.13341(11) 0.65436(11) 0.0396(3) Uani 1.000000 . . .
H69a H 1.13032(16) 0.09383(11) 0.65880(11) 0.0476(4) Uiso 1.000000 R . .
H69b H 1.02776(16) 0.14958(11) 0.58710(11) 0.0476(4) Uiso 1.000000 R . .
C70 C 1.11998(16) 0.22440(11) 0.71977(10) 0.0391(3) Uani 1.000000 . . .
H70a H 1.04663(16) 0.26153(11) 0.71958(10) 0.0470(4) Uiso 1.000000 R . .
H70b H 1.19433(16) 0.26528(11) 0.69750(10) 0.0470(4) Uiso 1.000000 R . .
N21 N 0.98407(15) 0.07574(12) 0.90446(11) 0.0453(3) Uani 1.000000 D . .
H21b H 0.985(3) 0.0695(17) 0.8441(16) 0.067(7) Uiso 1.000000 D . .
C21A C 1.00556(18) 0.00586(13) 1.05355(12) 0.0332(6) Uiso 0.773(6) D P 1
H59a H 0.59543(17) 0.20890(13) 0.90895(12) 0.0535(4) Uiso 1.000000 R . .
H59b H 0.70147(17) 0.19401(13) 1.00876(12) 0.0535(4) Uiso 1.000000 R . .
H60a H 0.71892(17) 0.04316(12) 0.94179(11) 0.0521(4) Uiso 1.000000 R . .
H60b H 0.56065(17) 0.04367(12) 0.94104(11) 0.0521(4) Uiso 1.000000 R . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
S 0.33376 0.55840 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.86690 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 7 -5 0.1108
-6 5 4 0.1072
-5 -3 6 0.0979
-4 -6 6 0.0983
5 -7 -2 0.0708
6 -3 -5 0.0726
-3 8 5 0.1036
-4 8 1 0.1063
1 -6 -7 0.0826
4 -8 -2 0.0751
5 -5 4 0.0885
-4 3 -5 0.1480
2 2 7 0.1347
-6 -3 3 0.1236
5 5 -2 0.1314
-4 5 7 0.1039
0 -4 8 0.1009
3 -4 -8 0.0570
-2 6 -6 0.1139
-2 -5 -5 0.0963
0 8 4 0.1152
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
C12A S11 C11 35.25(14) . . ?
C11A S12 C12 35.75(14) . . ?
H11b N11 H11a 121(3) . . ?
C11 N11 H11a 149.4(19) . . ?
C11 N11 H11b 89(2) . . ?
C11A N11 H11a 103.1(18) . . ?
C11A N11 H11b 135(2) . . ?
C11A N11 C11 46.70(18) . . ?
C11 H11b N11 63.3(18) . . ?
H12b N12 H12a 118(3) . . ?
C12 N12 H12a 153(2) . . ?
C12 N12 H12b 88(2) . . ?
C12A N12 H12a 104(2) . . ?
C12A N12 H12b 137(2) . . ?
C12A N12 C12 48.96(18) . . ?
C12 H12b N12 63.2(19) . . ?
N11 C11 S11 132.7(2) . . ?
H11b C11 S11 104.6(10) . . ?
H11b C11 N11 28.1(9) . . ?
C12 C11 S11 118.7(3) . . ?
C12 C11 N11 108.7(3) . . ?
C12 C11 H11b 136.7(10) . . ?
N12 C12 S12 134.3(3) . . ?
H12b C12 S12 105.9(10) . . ?
H12b C12 N12 28.4(10) . . ?
C11 C12 S12 118.3(3) . . ?
C11 C12 N12 107.4(3) . . ?
C11 C12 H12b 135.7(10) . . ?
N11 C11A S12 129.42(19) . . ?
C12A C11A S12 119.67(18) . . ?
C12A C11A N11 110.9(2) . . ?
N12 C12A S11 130.44(19) . . ?
C11A C12A S11 119.68(18) . . ?
C11A C12A N12 109.9(2) . . ?
C21A S21 C21 35.4(2) 2_757 . ?
C21 C21 S21 118.3(6) 2_757 . ?
H21a C21 S21 104.7(8) 2_757 . ?
N21 C21 S21 136.3(4) 2_757 . ?
N21 C21 H21a 31.7(7) 2_757 2_757 ?
N21 H21a C21 74.6(13) . 2_757 ?
C34 O31 C33 113.76(10) . . ?
C36 O32 C35 110.67(10) . . ?
C38 O33 C37 112.41(10) . . ?
H31b C31 H31a 108.0 . . ?
C32 C31 H31a 109.34(8) . . ?
C32 C31 H31b 109.34(8) . . ?
C40 C31 H31a 109.34(9) 2_666 . ?
C40 C31 H31b 109.34(8) 2_666 . ?
C40 C31 C32 111.45(13) 2_666 . ?
H32a C32 C31 109.61(8) . . ?
H32b C32 C31 109.61(8) . . ?
H32b C32 H32a 108.1 . . ?
C33 C32 C31 110.25(13) . . ?
C33 C32 H32a 109.61(8) . . ?
C33 C32 H32b 109.61(8) . . ?
C32 C33 O31 107.77(11) . . ?
H33 C33 O31 108.31(7) . . ?
H33 C33 C32 108.31(8) . . ?
C38 C33 O31 113.10(11) 2_666 . ?
C38 C33 C32 110.91(12) 2_666 . ?
C38 C33 H33 108.31(7) 2_666 . ?
H34a C34 O31 109.90(7) . . ?
H34b C34 O31 109.90(7) . . ?
H34b C34 H34a 108.3 . . ?
C35 C34 O31 108.91(12) . . ?
C35 C34 H34a 109.90(8) . . ?
C35 C34 H34b 109.90(8) . . ?
C34 C35 O32 109.01(11) . . ?
H35a C35 O32 109.88(7) . . ?
H35a C35 C34 109.88(8) . . ?
H35b C35 O32 109.88(7) . . ?
H35b C35 C34 109.88(8) . . ?
H35b C35 H35a 108.3 . . ?
H36a C36 O32 109.78(7) . . ?
H36b C36 O32 109.78(8) . . ?
H36b C36 H36a 108.2 . . ?
C37 C36 O32 109.48(12) . . ?
C37 C36 H36a 109.78(8) . . ?
C37 C36 H36b 109.78(8) . . ?
C36 C37 O33 108.56(11) . . ?
H37a C37 O33 109.98(7) . . ?
H37a C37 C36 109.98(8) . . ?
H37b C37 O33 109.98(8) . . ?
H37b C37 C36 109.98(8) . . ?
H37b C37 H37a 108.4 . . ?
C33 C38 O33 107.33(10) 2_666 . ?
H38 C38 O33 109.32(7) . . ?
H38 C38 C33 109.32(7) . 2_666 ?
C39 C38 O33 112.38(11) . . ?
C39 C38 C33 109.12(12) . 2_666 ?
C39 C38 H38 109.32(8) . . ?
H39a C39 C38 109.47(8) . . ?
H39b C39 C38 109.47(8) . . ?
H39b C39 H39a 108.1 . . ?
C40 C39 C38 110.87(12) . . ?
C40 C39 H39a 109.47(8) . . ?
C40 C39 H39b 109.47(8) . . ?
C39 C40 C31 110.89(13) . 2_666 ?
H40a C40 C31 109.46(9) . 2_666 ?
H40a C40 C39 109.46(8) . . ?
H40b C40 C31 109.46(8) . 2_666 ?
H40b C40 C39 109.46(8) . . ?
H40b C40 H40a 108.1 . . ?
C70 O51 C51 113.65(11) . . ?
C57 O52 C56 113.00(11) . . ?
C59 O53 C58 111.32(12) . . ?
C61 O54 C60 113.33(11) . . ?
C67 O55 C66 113.51(11) . . ?
C69 O56 C68 111.08(11) . . ?
H51 C51 O51 108.16(7) . . ?
C52 C51 O51 107.51(12) . . ?
C52 C51 H51 108.16(8) . . ?
C56 C51 O51 112.97(12) . . ?
C56 C51 H51 108.16(7) . . ?
C56 C51 C52 111.74(12) . . ?
H52a C52 C51 109.60(8) . . ?
H52b C52 C51 109.60(9) . . ?
H52b C52 H52a 108.1 . . ?
C53 C52 C51 110.29(13) . . ?
C53 C52 H52a 109.60(9) . . ?
C53 C52 H52b 109.60(9) . . ?
H53a C53 C52 109.59(9) . . ?
H53b C53 C52 109.59(9) . . ?
H53b C53 H53a 108.1 . . ?
C54 C53 C52 110.32(13) . . ?
C54 C53 H53a 109.59(9) . . ?
C54 C53 H53b 109.59(10) . . ?
H54a C54 C53 109.41(10) . . ?
H54b C54 C53 109.41(9) . . ?
H54b C54 H54a 108.0 . . ?
C55 C54 C53 111.12(14) . . ?
C55 C54 H54a 109.41(9) . . ?
C55 C54 H54b 109.41(9) . . ?
H55a C55 C54 109.28(9) . . ?
H55b C55 C54 109.28(9) . . ?
H55b C55 H55a 107.9 . . ?
C56 C55 C54 111.70(13) . . ?
C56 C55 H55a 109.28(8) . . ?
C56 C55 H55b 109.28(9) . . ?
C51 C56 O52 107.95(11) . . ?
C55 C56 O52 111.17(12) . . ?
C55 C56 C51 110.22(13) . . ?
H56 C56 O52 109.15(7) . . ?
H56 C56 C51 109.15(8) . . ?
H56 C56 C55 109.15(8) . . ?
H57a C57 O52 109.76(8) . . ?
H57b C57 O52 109.76(7) . . ?
H57b C57 H57a 108.2 . . ?
C58 C57 O52 109.55(12) . . ?
C58 C57 H57a 109.76(8) . . ?
C58 C57 H57b 109.76(8) . . ?
C57 C58 O53 109.54(12) . . ?
H58a C58 O53 109.77(8) . . ?
H58a C58 C57 109.77(8) . . ?
H58b C58 O53 109.77(8) . . ?
H58b C58 C57 109.77(8) . . ?
H58b C58 H58a 108.2 . . ?
C60 C59 O53 110.00(13) . . ?
H59a C59 O53 109.66(8) . . ?
H59a C59 C60 109.66(9) . . ?
H59b C59 O53 109.66(8) . . ?
H59b C59 C60 109.66(9) . . ?
H59b C59 H59a 108.2 . . ?
C59 C60 O54 109.38(13) . . ?
H60a C60 O54 109.80(8) . . ?
H60a C60 C59 109.80(9) . . ?
H60b C60 O54 109.80(7) . . ?
H60b C60 C59 109.80(8) . . ?
H60b C60 H60a 108.2 . . ?
H61 C61 O54 109.71(7) . . ?
C62 C61 O54 112.13(13) . . ?
C62 C61 H61 109.71(9) . . ?
C66 C61 O54 106.74(11) . . ?
C66 C61 H61 109.71(8) . . ?
C66 C61 C62 108.78(12) . . ?
H62a C62 C61 109.49(9) . . ?
H62b C62 C61 109.49(9) . . ?
H62b C62 H62a 108.1 . . ?
C63 C62 C61 110.77(13) . . ?
C63 C62 H62a 109.49(9) . . ?
C63 C62 H62b 109.49(9) . . ?
H63a C63 C62 109.54(8) . . ?
H63b C63 C62 109.54(9) . . ?
H63b C63 H63a 108.1 . . ?
C64 C63 C62 110.54(14) . . ?
C64 C63 H63a 109.54(8) . . ?
C64 C63 H63b 109.54(9) . . ?
H64a C64 C63 109.34(9) . . ?
H64b C64 C63 109.34(9) . . ?
H64b C64 H64a 108.0 . . ?
C65 C64 C63 111.44(13) . . ?
C65 C64 H64a 109.34(9) . . ?
C65 C64 H64b 109.34(9) . . ?
H65a C65 C64 109.71(9) . . ?
H65b C65 C64 109.71(9) . . ?
H65b C65 H65a 108.2 . . ?
C66 C65 C64 109.78(13) . . ?
C66 C65 H65a 109.71(8) . . ?
C66 C65 H65b 109.71(8) . . ?
C61 C66 O55 112.37(11) . . ?
C65 C66 O55 108.22(11) . . ?
C65 C66 C61 111.87(13) . . ?
H66 C66 O55 108.08(7) . . ?
H66 C66 C61 108.08(8) . . ?
H66 C66 C65 108.08(8) . . ?
H67a C67 O55 109.86(9) . . ?
H67b C67 O55 109.86(8) . . ?
H67b C67 H67a 108.3 . . ?
C68 C67 O55 109.11(12) . . ?
C68 C67 H67a 109.86(9) . . ?
C68 C67 H67b 109.86(9) . . ?
C67 C68 O56 109.70(13) . . ?
H68a C68 O56 109.73(8) . . ?
H68a C68 C67 109.73(9) . . ?
H68b C68 O56 109.73(7) . . ?
H68b C68 C67 109.73(8) . . ?
H68b C68 H68a 108.2 . . ?
H69a C69 O56 109.83(8) . . ?
H69b C69 O56 109.83(7) . . ?
H69b C69 H69a 108.3 . . ?
C70 C69 O56 109.26(12) . . ?
C70 C69 H69a 109.83(9) . . ?
C70 C69 H69b 109.83(8) . . ?
C69 C70 O51 108.48(12) . . ?
H70a C70 O51 110.00(8) . . ?
H70a C70 C69 110.00(8) . . ?
H70b C70 O51 110.00(7) . . ?
H70b C70 C69 110.00(8) . . ?
H70b C70 H70a 108.4 . . ?
H21a N21 C21 73.8(13) . 2_757 ?
H21b N21 C21 159.1(16) . 2_757 ?
H21b N21 H21a 127(2) . . ?
C21A N21 C21 47.7(3) 2_757 2_757 ?
C21A N21 H21a 121.4(13) 2_757 . ?
C21A N21 H21b 111.7(16) 2_757 . ?
N21 C21A S21 126.80(14) 2_757 2_757 ?
C21A C21A S21 120.74(17) 2_757 2_757 ?
C21A C21A N21 112.45(19) 2_757 2_757 ?
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
S11 C11 1.721(3) . ?
S11 C12A 1.680(2) . ?
S12 C12 1.684(3) . ?
S12 C11A 1.698(2) . ?
N11 H11a 0.83(3) . ?
N11 H11b 0.72(3) . ?
N11 C11 1.370(4) . ?
N11 C11A 1.342(3) . ?
H11b C11 1.53(2) . ?
N12 H12a 0.82(3) . ?
N12 H12b 0.73(3) . ?
N12 C12 1.377(4) . ?
N12 C12A 1.352(3) . ?
H12b C12 1.54(3) . ?
C11 C12 1.509(5) . ?
C11A C12A 1.515(3) . ?
S21 C21 1.709(6) . ?
S21 C21A 1.6760(18) 2_757 ?
C21 C21 1.503(12) 2_757 ?
C21 H21a 1.408(18) 2_757 ?
C21 N21 1.414(6) 2_757 ?
H21a N21 0.770(16) . ?
O31 C33 1.4257(16) . ?
O31 C34 1.4157(17) . ?
O32 C35 1.4227(17) . ?
O32 C36 1.4270(16) . ?
O33 C37 1.4220(17) . ?
O33 C38 1.4281(16) . ?
C31 H31a 0.9900 . ?
C31 H31b 0.9900 . ?
C31 C32 1.533(2) . ?
C31 C40 1.524(2) 2_666 ?
C32 H32a 0.9900 . ?
C32 H32b 0.9900 . ?
C32 C33 1.519(2) . ?
C33 H33 1.0000 . ?
C33 C38 1.5287(19) 2_666 ?
C34 H34a 0.9900 . ?
C34 H34b 0.9900 . ?
C34 C35 1.5017(19) . ?
C35 H35a 0.9900 . ?
C35 H35b 0.9900 . ?
C36 H36a 0.9900 . ?
C36 H36b 0.9900 . ?
C36 C37 1.500(2) . ?
C37 H37a 0.9900 . ?
C37 H37b 0.9900 . ?
C38 H38 1.0000 . ?
C38 C39 1.5294(19) . ?
C39 H39a 0.9900 . ?
C39 H39b 0.9900 . ?
C39 C40 1.522(2) . ?
C40 H40a 0.9900 . ?
C40 H40b 0.9900 . ?
O51 C51 1.4252(17) . ?
O51 C70 1.4189(17) . ?
O52 C56 1.4317(17) . ?
O52 C57 1.4179(18) . ?
O53 C58 1.4187(18) . ?
O53 C59 1.4183(18) . ?
O54 C60 1.4210(18) . ?
O54 C61 1.4328(18) . ?
O55 C66 1.4297(17) . ?
O55 C67 1.4128(18) . ?
O56 C68 1.4216(17) . ?
O56 C69 1.4290(17) . ?
C51 H51 1.0000 . ?
C51 C52 1.523(2) . ?
C51 C56 1.527(2) . ?
C52 H52a 0.9900 . ?
C52 H52b 0.9900 . ?
C52 C53 1.533(2) . ?
C53 H53a 0.9900 . ?
C53 H53b 0.9900 . ?
C53 C54 1.522(3) . ?
C54 H54a 0.9900 . ?
C54 H54b 0.9900 . ?
C54 C55 1.529(2) . ?
C55 H55a 0.9900 . ?
C55 H55b 0.9900 . ?
C55 C56 1.528(2) . ?
C56 H56 1.0000 . ?
C57 H57a 0.9900 . ?
C57 H57b 0.9900 . ?
C57 C58 1.501(2) . ?
C58 H58a 0.9900 . ?
C58 H58b 0.9900 . ?
C59 C60 1.501(2) . ?
C59 H59a 0.9900 . ?
C59 H59b 0.9900 . ?
C60 H60a 0.9900 . ?
C60 H60b 0.9900 . ?
C61 H61 1.0000 . ?
C61 C62 1.533(2) . ?
C61 C66 1.530(2) . ?
C62 H62a 0.9900 . ?
C62 H62b 0.9900 . ?
C62 C63 1.528(3) . ?
C63 H63a 0.9900 . ?
C63 H63b 0.9900 . ?
C63 C64 1.521(2) . ?
C64 H64a 0.9900 . ?
C64 H64b 0.9900 . ?
C64 C65 1.530(2) . ?
C65 H65a 0.9900 . ?
C65 H65b 0.9900 . ?
C65 C66 1.519(2) . ?
C66 H66 1.0000 . ?
C67 H67a 0.9900 . ?
C67 H67b 0.9900 . ?
C67 C68 1.496(2) . ?
C68 H68a 0.9900 . ?
C68 H68b 0.9900 . ?
C69 H69a 0.9900 . ?
C69 H69b 0.9900 . ?
C69 C70 1.498(2) . ?
C70 H70a 0.9900 . ?
C70 H70b 0.9900 . ?
N21 H21b 0.88(2) . ?
N21 C21A 1.330(2) 2_757 ?
C21A C21A 1.529(3) 2_757 ?
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
S11 C11 N11 C11A 176.9(5) . . . . ?
S11 C11 C12 S12 -176.48(19) . . . . ?
S11 C11 C12 N12 5.0(2) . . . . ?
S11 C12A N12 C12 -177.9(4) . . . . ?
S11 C12A C11A S12 176.90(14) . . . . ?
S11 C12A C11A N11 -5.60(19) . . . . ?
S12 C12 N12 C12A -180.0(5) . . . . ?
S12 C12 C11 N11 2.7(3) . . . . ?
S12 C11A N11 C11 178.7(4) . . . . ?
S12 C11A C12A N12 -2.39(19) . . . . ?
N11 C11 C12 N12 -175.9(2) . . . . ?
N11 C11A C12A N12 175.11(19) . . . . ?
S21 C21 C21 S21 -180.0(5) . . 2_757 2_757 ?
S21 C21 C21 N21 -0.2(4) . . 2_757 . ?
S21 C21 N21 C21A 179.9(8) . . 2_757 . ?
S21 C21A N21 C21 -179.6(4) . 2_757 . 2_757 ?
S21 C21A C21A S21 180.00(14) . 2_757 . 2_757 ?
S21 C21A C21A N21 -0.65(14) . 2_757 . 2_757 ?
C21 C21 N21 C21A 0.3(4) . 2_757 . 2_757 ?
C21 N21 C21A C21A 0.3(4) . 2_757 . 2_757 ?
O31 C33 C32 C31 -177.90(11) . . . . ?
O31 C33 C38 O33 -58.56(12) . . 2_666 2_666 ?
O31 C33 C38 C39 179.42(11) . . 2_666 2_666 ?
O31 C34 C35 O32 -64.03(12) . . . . ?
O32 C36 C37 O33 -64.53(12) . . . . ?
O33 C38 C33 C32 -62.65(12) . . 2_666 2_666 ?
O33 C38 C39 C40 60.33(13) . . . . ?
C31 C32 C33 C38 57.80(13) . . . 2_666 ?
C31 C40 C39 C38 56.81(13) 2_666 . . . ?
C32 C33 C38 C39 -59.38(12) . . 2_666 2_666 ?
C33 C38 C39 C40 -58.59(12) 2_666 . . . ?
O51 C51 C52 C53 178.04(12) . . . . ?
O51 C51 C56 O52 55.57(12) . . . . ?
O51 C51 C56 C55 177.16(12) . . . . ?
O51 C70 C69 O56 65.55(12) . . . . ?
O52 C56 C51 C52 -65.82(12) . . . . ?
O52 C56 C55 C54 65.05(14) . . . . ?
O52 C57 C58 O53 -60.78(13) . . . . ?
O53 C59 C60 O54 -62.50(13) . . . . ?
O54 C61 C62 C63 59.88(14) . . . . ?
O54 C61 C66 O55 59.32(12) . . . . ?
O54 C61 C66 C65 -62.65(12) . . . . ?
O55 C66 C61 C62 -179.50(13) . . . . ?
O55 C66 C65 C64 178.20(12) . . . . ?
O55 C67 C68 O56 65.40(14) . . . . ?
C51 C52 C53 C54 57.39(14) . . . . ?
C51 C56 C55 C54 -54.62(13) . . . . ?
C52 C53 C54 C55 -56.73(15) . . . . ?
C53 C54 C55 C56 55.86(15) . . . . ?
C61 C62 C63 C64 57.64(15) . . . . ?
C61 C66 C65 C64 -57.48(13) . . . . ?
C62 C63 C64 C65 -56.37(14) . . . . ?
C63 C64 C65 C66 55.86(15) . . . . ?
N21 C21A C21A N21 -180.0(2) . 2_757 . 2_757 ?
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
H21a N21 1 0.8900 0.0400 0.1201
H21b N21 1 0.8900 0.0400 0.0108
loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
S11 C11 1 1
S11 C12 1 6
S11 C11A 1 1
S11 C12A 1 6
S12 C11 1 8
S12 C12 1 2
S12 C11A 1 8
S12 C12A 1 2
N11 C11 1 3
N11 C12 1 4
N11 C11A 1 3
N11 C12A 1 4
N12 C11 1 9
N12 C12 1 5
N12 C11A 1 9
N12 C12A 1 5
C11 C12 1 7
C11A C12A 1 7
S21 C21 1 10
S21 C21A 1 10
N21 C21 1 11
N21 C21A 1 11
loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0200 2.2424 0.5212 0.5212
2 0.0200 2.2313 0.5476 0.5476
3 0.0200 1.3562 0.0142 0.0142
4 0.0400 2.3475 0.0069 0.0069
5 0.0200 1.3643 0.0124 0.0124
6 0.0400 2.2303 0.5503 0.5503
7 0.0200 1.5119 0.0029 0.0029
8 0.0400 2.2201 0.5224 0.5224
9 0.0400 2.3377 0.0106 0.0106
10 0.0200 2.2480 0.5388 0.5388
11 0.0200 2.3502 0.0287 0.0287
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.2405 7.1403 -4.9678 -0.2076 -0.8658 0.4554
-6.0308 4.8489 3.6828 0.1206 0.5057 0.8542
-5.0687 -3.0828 5.9769 0.2317 0.9677 0.0994
-3.5088 -5.7411 5.5895 0.2261 0.9433 -0.2429
5.1914 -6.9160 -2.0664 -0.0539 -0.2274 -0.9723
6.2935 -2.5626 -4.8486 -0.1714 -0.7171 -0.6756
-2.5107 7.8904 4.5098 -0.5240 0.1262 0.8423
-4.1384 8.1243 0.9940 -0.0394 0.0102 0.9992
0.5527 -5.9637 -6.5683 0.8292 -0.1990 -0.5224
3.6017 -8.3074 -2.4964 0.2431 -0.0590 -0.9682
4.5299 -5.1390 3.8637 -0.5908 0.1409 -0.7944
-4.0565 3.0874 -5.4579 0.7848 -0.1875 0.5907
2.1187 1.7135 7.2380 -0.9716 0.2327 -0.0433
-5.8611 -2.5246 2.5581 0.5933 0.7743 0.2201
4.6571 5.1108 -2.3917 -0.6059 -0.7904 0.0900
-3.8201 5.2718 7.1008 -0.4584 0.5355 0.7093
0.4952 -3.6112 8.4234 -0.6018 0.7042 -0.3767
3.4139 -4.1857 -8.0230 0.5284 -0.6174 -0.5827
-2.2218 6.2388 -5.9955 0.4499 -0.5269 0.7211
-1.9466 -5.3363 -5.0691 0.9554 0.0759 -0.2855
-0.4929 7.8250 4.1750 -0.7261 -0.0580 0.6851
