Towards the stable chelation of radium for biomedical applications with an 18-membered macrocyclic ligand
Abou, Diane S.; Thiele, Nikki A.; Gutsche, Nicholas T.; Villmer, Alexandria; Zhang, Hanwen; Woods, Joshua J.; Baidoo, Kwamena E.; Escorcia, Freddy E.; Wilson, Justin J.; Thorek, Daniel L. J.; Chemical Science 12 (2021) 3733–3742; doi:10.1039/D0SC06867E

data_1560236
_publ_section_title
;
 Towards the stable chelation of radium for biomedical applications with
 an 18-membered macrocyclic ligand
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3733
_journal_page_last               3742
_journal_paper_doi               10.1039/D0SC06867E
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C32 H43 Ba N6 O11 S2'
_chemical_formula_sum            'C32 H43 Ba N6 O11 S2'
_chemical_formula_weight         889.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-04
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2020-10-01 deposited with the CCDC.	2021-01-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.68270(10)
_cell_length_b                   10.44220(10)
_cell_length_c                   22.5408(2)
_cell_measurement_reflns_used    88251
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      76.8540
_cell_measurement_theta_min      3.9280
_cell_volume                     4162.08(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.63a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     31.00  61.00   0.50    0.29    --   50.06  77.00  90.00   60
  2  \w     49.00  97.00   0.50    0.29    --   66.00  71.00  81.83   96
  3  \w     55.00  81.00   0.50    0.29    --   74.00  75.00 106.42   52
  4  \w     86.00 113.00   0.50    1.14    --  102.00  68.00 124.51   54
  5  \w    126.00 172.00   0.50    1.14    --  104.00  77.00  90.00   92
  6  \w    141.00 166.00   0.50    1.14    --  102.00  68.00 124.51   50
  7  \w    148.00 174.00   0.50    1.14    --  104.00  77.00 120.00   52
  8  \w    135.00 162.00   0.50    1.14    --  104.00  61.00 120.00   54
  9  \w    142.00 172.00   0.50    1.14    --  104.00  35.00 157.49   60
 10  \w    121.00 173.00   0.50    1.14    --  104.00  77.00 150.00  104
 11  \w    144.00 169.00   0.50    1.14    --  104.00  45.00  30.00   50
 12  \w    150.00 176.00   0.50    1.14    --  104.00  77.00 -30.00   52
 13  \w    138.00 175.00   0.50    1.14    --  104.00  77.00 -90.00   74
 14  \w    146.00 172.00   0.50    1.14    --  104.00  77.00-150.00   52
 15  \w    131.00 163.00   0.50    1.14    --   98.00  76.00-132.82   64
 16  \w    139.00 170.00   0.50    1.14    --  104.00  77.00-180.00   62
 17  \w    134.00 165.00   0.50    1.14    --  104.00  45.00-180.00   62
 18  \w    127.00 161.00   0.50    1.14    --  104.00  79.00-163.39   68
 19  \w    127.00 165.00   0.50    1.14    --  104.00 102.00 -79.00   76
 20  \w    147.00 173.00   0.50    1.14    --  104.00 125.00 -60.00   52
 21  \w    124.00 156.00   0.50    1.14    --  104.00  61.00 -90.00   64
 22  \w    115.00 141.00   0.50    1.14    --  104.00  77.00 -60.00   52
 23  \w    124.00 161.00   0.50    1.14    --  104.00  61.00   0.00   74
 24  \w    132.00 176.00   0.50    1.14    --  104.00  77.00  30.00   88
 25  \w    127.00 153.00   0.50    1.14    --  104.00  61.00  30.00   52
 26  \w    114.00 164.00   0.50    1.14    --  104.00  30.00  60.00  100
 27  \w    111.00 171.00   0.50    1.14    --  104.00  30.00 150.00  120
 28  \w    110.00 138.00   0.50    1.14    --  104.00  35.00 157.49   56
 29  \w    109.00 158.00   0.50    1.14    --  104.00  61.00 150.00   98
 30  \w     92.00 139.00   0.50    1.14    --  104.00  61.00  90.00   94
 31  \w     98.00 130.00   0.50    1.14    --  104.00  45.00  30.00   64
 32  \w     91.00 166.00   0.50    1.14    --  104.00  61.00  60.00  150
 33  \w    100.00 147.00   0.50    1.14    --  104.00  45.00 -60.00   94
 34  \w    107.00 163.00   0.50    1.14    --  104.00  45.00-120.00  112
 35  \w    115.00 171.00   0.50    1.14    --  104.00 125.00-180.00  112
 36  \w    105.00 131.00   0.50    1.14    --  104.00  45.00-180.00   52
 37  \w    102.00 150.00   0.50    1.14    --  104.00  61.00-120.00   96
 38  \w     96.00 175.00   0.50    1.14    --  104.00  45.00 -30.00  158
 39  \w     98.00 138.00   0.50    1.14    --  104.00 125.00 -60.00   80
 40  \w    102.00 158.00   0.50    1.14    --  104.00 125.00 -30.00  112
 41  \w     91.00 118.00   0.50    1.14    --  104.00  61.00 -90.00   54
 42  \w     91.00 135.00   0.50    1.14    --  104.00  61.00-150.00   88
 43  \w     91.00 167.00   0.50    1.14    --  104.00  61.00-180.00  152
 44  \w     85.00 111.00   0.50    0.29    --   58.00  79.00-147.96   52
 45  \w     79.00 105.00   0.50    1.14    --   98.00  76.00-132.82   52
 46  \w     86.00 133.00   0.50    1.14    --  104.00  77.00-150.00   94
 47  \w     85.00 175.00   0.50    1.14    --  104.00  77.00-120.00  180
 48  \w     92.00 138.00   0.50    1.14    --  104.00  61.00 -30.00   92
 49  \w     85.00 120.00   0.50    1.14    --  104.00  77.00 -30.00   70
 50  \w     91.00 121.00   0.50    1.14    --  104.00  61.00  30.00   60
 51  \w     91.00 118.00   0.50    1.14    --  104.00  61.00   0.00   54
 52  \w     91.00 137.00   0.50    1.14    --  104.00  61.00 -60.00   92
 53  \w     85.00 132.00   0.50    1.14    --  104.00  77.00   0.00   94
 54  \w     85.00 111.00   0.50    1.14    --  104.00  77.00  90.00   52
 55  \w     85.00 111.00   0.50    1.14    --  104.00  77.00 150.00   52
 56  \w     85.00 112.00   0.50    1.14    --  104.00  77.00 120.00   54
 57  \w     85.00 148.00   0.50    1.14    --  104.00  77.00  60.00  126
 58  \w     91.00 121.00   0.50    1.14    --  104.00  61.00 120.00   60
 59  \w     85.00 128.00   0.50    1.14    --  104.00  77.00  30.00   86
 60  \w     85.00 111.00   0.50    1.14    --  104.00  77.00 -60.00   52
 61  \w     85.00 131.00   0.50    1.14    --  104.00  77.00 -90.00   92
 62  \w     85.00 113.00   0.50    1.14    --  104.00  77.00-180.00   56
 63  \w     84.00 111.00   0.50    1.14    --  104.00  79.00-163.39   54
 64  \w     79.00 105.00   0.50    1.14    --  104.00   0.00-180.00   52
 65  \w     49.00  74.00   0.50    0.29    --   66.00  74.00-172.78   50
 66  \w     58.00  84.00   0.50    0.29    --   42.00  79.00-173.72   52
 67  \w     32.00  63.00   0.50    0.29    --   50.06  77.00 -60.00   62
 68  \w     34.00  67.00   0.50    0.29    --   54.00  79.00-110.38   66
 69  \w     36.00  61.00   0.50    0.29    --   54.00  76.00-153.96   50
 70  \w     38.00  64.00   0.50    0.29    --   58.00  79.00-147.96   52
 71  \w     23.00  50.00   0.50    0.29    --   42.00  79.00-173.72   54
 72  \w     17.00  42.00   0.50    0.29    --   42.00  89.00-108.53   50
 73  \w      0.00  29.00   0.50    0.29    --   26.00  96.00 -75.29   58
 74  \w     -9.00  18.00   0.50    0.29    --   22.00 101.00  10.70   54
 75  \w     17.00  42.00   0.50    0.29    --   42.00  90.00   4.12   50
 76  \w     34.00  91.00   0.50    0.29    --   54.00  80.00  33.62  114
 77  \w     39.00  65.00   0.50    0.29    --   58.00  75.00 116.48   52
 78  \w     35.00  66.00   0.50    0.29    --   54.00  77.00 172.41   62
 79  \w     47.00  78.00   0.50    0.29    --   66.00  75.00 154.96   62
 80  \w     44.00  82.00   0.50    0.29    --   62.00  76.00 130.53   76
 81  \w     30.00  56.00   0.50    0.29    --   50.00  80.00 139.95   52
 82  \w     16.00  41.00   0.50    0.29    --   42.00  91.00  81.35   50
 83  \w     42.00  68.00   0.50    0.29    --   62.00  78.00  -5.32   52
 84  \w     40.00  65.00   0.50    0.29    --   58.00  75.00 -15.13   50
 85  \w    -17.00  18.00   0.50    0.29    --   14.00 101.00  54.61   70
 86  \w    -25.00   0.00   0.50    0.29    --   10.00 107.00 117.86   50
 87  \w    -81.00 -30.00   0.50    0.29    --  -50.06 102.00 -79.00  102
 88  \w    -24.00   2.00   0.50    0.29    --  -50.06 102.00 -79.00   52
 89  \w    -43.00 -16.00   0.50    0.29    --   -2.00 131.00-144.83   54
 90  \w    -54.00 -27.00   0.50    0.29    --    6.00 152.00-115.50   54
 91  \w    -51.00  30.00   0.50    0.29    --  -38.00  61.00-176.52  162
 92  \w    -67.00 -42.00   0.50    1.14    --  -82.50 102.00 -79.00   50
 93  \w    -60.00 -33.00   0.50    0.29    --  -54.00 -79.00 -48.70   54
 94  \w    -77.00 -41.00   0.50    0.29    --  -62.00 -80.00 -63.41   72
 95  \w    -83.00 -45.00   0.50    0.29    --  -66.00 -80.00 -91.12   76
 96  \w    -85.00 -59.00   0.50    1.14    --  -78.00 -75.00-142.06   52
 97  \w   -100.00 -63.00   0.50    1.14    --  -82.50 -76.00 -78.50   74
 98  \w    -85.00 -59.00   0.50    1.14    --  -78.00 -75.00 -44.78   52
 99  \w    -86.00 -60.00   0.50    1.14    --  -78.00 -72.00  -2.28   52
100  \w    -72.00 -46.00   0.50    0.29    --  -66.00 -77.00  32.89   52
101  \w    -69.00 -43.00   0.50    0.29    --  -62.00 -76.00  65.36   52
102  \w    -87.00 -60.00   0.50    1.14    --  -78.00 -74.00  29.12   54
103  \w    -89.00 -63.00   0.50    1.14    --  -82.50 -76.00  66.97   52
104  \w    -93.00 -60.00   0.50    1.14    --  -78.00 -72.00  10.83   66
105  \w    -89.00 -63.00   0.50    1.14    --  -82.50 -79.00  24.43   52
106  \w    -91.00 -65.00   0.50    1.14    --  -82.50 -74.00 -22.04   52
107  \w    -89.00 -63.00   0.50    1.14    --  -82.50 -77.00 -60.00   52
108  \w    -94.00 -63.00   0.50    1.14    --  -82.50 -77.00   0.00   62
109  \w    -93.00 -66.00   0.50    1.14    --  -82.50 -69.00 -18.69   54
110  \w    -96.00 -64.00   0.50    1.14    --  -82.50 -73.00  49.63   64
111  \w   -102.00 -64.00   0.50    1.14    --  -82.50 -77.00  88.94   76
112  \w    -93.00 -64.00   0.50    1.14    --  -82.50 -74.00 123.66   58
113  \w    -88.00 -61.00   0.50    1.14    --  -82.50 -80.00 175.17   54
114  \w    -92.00 -66.00   0.50    1.14    --  -82.50 -69.00 131.24   52
115  \w    -96.00 -63.00   0.50    1.14    --  -82.50 -77.00 120.00   66
116  \w    -99.00 -63.00   0.50    1.14    --  -82.50 -76.00 155.81   72
117  \w   -121.00 -62.00   0.50    1.14    --  -82.50 -78.00  97.16  118
118  \w   -144.00-119.00   0.50    1.14    --  -82.50-102.00 177.00   50
119  \w   -136.00-109.00   0.50    1.14    --  -78.00 -75.00 -44.78   54
120  \w   -117.00 -92.00   0.50    0.29    --  -66.00 -80.00 -91.12   50
121  \w   -104.00 -62.00   0.50    1.14    --  -82.50 -78.00 -92.99   84
122  \w    -92.00 -65.00   0.50    1.14    --  -82.50 -77.00-180.00   54
123  \w   -113.00 -62.00   0.50    1.14    --  -82.50 -79.00-150.03  102
124  \w   -153.00 -64.00   0.50    1.14    --  -82.50 -77.00-108.89  178
125  \w     35.00  95.00   0.50    0.29    --   50.06-125.00 -60.00  120
126  \w     50.00 106.00   0.50    1.14    --  104.00-100.00   9.68  112
127  \w    101.00 127.00   0.50    1.14    --  104.00 -86.00 -21.67   52
128  \w     97.00 123.00   0.50    1.14    --  104.00 -84.00 -53.32   52
129  \w     80.00 106.00   0.50    1.14    --  104.00-100.00 -26.43   52
130  \w     75.00 112.00   0.50    1.14    --  104.00-125.00 -60.00   74
131  \w     83.00 111.00   0.50    1.14    --  104.00 -83.00   3.72   56
132  \w     91.00 116.00   0.50    1.14    --  104.00 -80.00  33.49   50
133  \w     76.00 111.00   0.50    1.14    --  104.00-125.00 -30.00   70
134  \w     74.00 101.00   0.50    1.14    --  104.00 -77.00 -60.00   54
135  \w     78.00 104.00   0.50    1.14    --  104.00 -94.00 -60.00   52
136  \w     78.00 112.00   0.50    1.14    --  104.00-125.00 -90.00   68
137  \w     80.00 106.00   0.50    1.14    --  104.00 -94.00-150.00   52
138  \w     79.00 112.00   0.50    1.14    --  104.00-125.00-180.00   66
139  \w     43.00  68.00   0.50    1.14    --  104.00-125.00 -60.00   50
140  \w     38.00  69.00   0.50    1.14    --  104.00-125.00 -90.00   62
141  \w     41.00  71.00   0.50    1.14    --  104.00-100.00 -26.43   60
142  \w     33.00 106.00   0.50    1.14    --  104.00 -94.00 -90.00  146
143  \w     53.00 100.00   0.50    1.14    --  104.00 -77.00-180.00   94
144  \w     36.00 108.00   0.50    1.14    --  104.00-125.00-150.00  144
145  \w     39.00  69.00   0.50    1.14    --  104.00 -77.00 -60.00   60
146  \w     38.00  79.00   0.50    1.14    --  104.00 -86.00 -21.67   82
147  \w     35.00  68.00   0.50    1.14    --  104.00-125.00 -30.00   66
148  \w     38.00  78.00   0.50    1.14    --  104.00 -83.00   3.72   80
149  \w     39.00  64.00   0.50    1.14    --  104.00-125.00  90.00   50
150  \w     66.00  92.00   0.50    1.14    --  104.00-125.00  90.00   52
151  \w     80.00 112.00   0.50    1.14    --  104.00-125.00 150.00   64
152  \w     81.00 106.00   0.50    1.14    --  104.00 -94.00 120.00   50
153  \w     76.00 101.00   0.50    1.14    --  104.00 -77.00 150.00   50
154  \w     59.00 107.00   0.50    1.14    --  104.00-102.00 177.00   96
155  \w     63.00 105.00   0.50    1.14    --  104.00 -77.00  70.45   84
156  \w     36.00  65.00   0.50    1.14    --  104.00 -94.00 120.00   58
157  \w     34.00  60.00   0.50    1.14    --  104.00-125.00 150.00   52
158  \w     36.00 112.00   0.50    1.14    --  104.00-125.00 120.00  152
159  \w     33.00  68.00   0.50    1.14    --  104.00 -61.00   0.00   70
160  \w     39.00  78.00   0.50    1.14    --  104.00 -80.00  33.49   78
161  \w     34.00  71.00   0.50    1.14    --  104.00 -61.00  90.00   74
162  \w     33.00  58.00   0.50    1.14    --  104.00 -61.00 150.00   50
163  \w     32.00  68.00   0.50    1.14    --  104.00 -94.00 150.00   72
164  \w      8.00  74.00   0.50    0.29    --   50.06-102.00 177.00  132
165  \w     33.00  66.00   0.50    1.14    --  104.00 -84.00 -53.32   66
166  \w     35.00  61.00   0.50    1.14    --  104.00 -94.00 -60.00   52
167  \w     33.00  76.00   0.50    1.14    --  104.00 -77.00-120.00   86
168  \w     33.00  68.00   0.50    1.14    --  104.00 -61.00-150.00   70
169  \w     32.00  60.00   0.50    1.14    --  104.00 -61.00-180.00   56
170  \w     37.00  62.00   0.50    1.14    --  104.00-125.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0425767000
_diffrn_orient_matrix_UB_12      -0.0894657000
_diffrn_orient_matrix_UB_13      0.0429075000
_diffrn_orient_matrix_UB_21      0.0569516000
_diffrn_orient_matrix_UB_22      0.0327048000
_diffrn_orient_matrix_UB_23      0.0494378000
_diffrn_orient_matrix_UB_31      -0.0503121000
_diffrn_orient_matrix_UB_32      0.1126652000
_diffrn_orient_matrix_UB_33      0.0196816000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            191674
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         1.960
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.63a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.052
_refine_diff_density_max         2.443
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 3626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         7895
_refine_ls_number_restraints     693
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0698
_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/[\s^2^(Fo^2^)+(0.1546P)^2^+4.4472P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2009
_refine_ls_wR_factor_ref         0.2018
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7765
_reflns_number_total             7895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06867e2.cif
_cod_data_source_block           '[Ba(Macropa)-beta-ala]'
_cod_depositor_comments          'Adding full bibliography for 1560236.cif.'
_cod_database_code               1560236
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ba C30 N6 O4'
_chemical_oxdiff_usercomment     'Grown from D6-DMSO'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.628
 0.372
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
3. Restrained distances
 C26-C25A \\sim C25B-C26
 with sigma of 0.02
 C25B-C24B \\sim C24A-C25A
 with sigma of 0.02
 N29-C25B \\sim N4-C25A
 with sigma of 0.02
 N29-C21B \\sim N4-C21A
 with sigma of 0.02
 C21B-C22B \\sim C22A-C21A
 with sigma of 0.02
 C22B-C23B \\sim C23A-C22A
 with sigma of 0.02
 C24A-C23A \\sim C24B-C23B
 with sigma of 0.02
 N5A-C23A \\sim N5B-C23B
 with sigma of 0.02
 N5B-C27B \\sim N5A-C27A
 with sigma of 0.02
 S1B-C27B \\sim S1A-C27A
 with sigma of 0.02
 N6B-C27B \\sim N6A-C27A
 with sigma of 0.02
 N6B-C28B \\sim N6A-C28A
 with sigma of 0.02
 C28B-C29B \\sim C28A-C29A
 with sigma of 0.02
 C30-C29A \\sim C29B-C30
 with sigma of 0.02
 O11B-C30 \\sim O11A-C30
 with sigma of 0.02
 O10A-C30 \\sim O10B-C30
 with sigma of 0.02
 C3B-C2 \\sim C3A-C2
 with sigma of 0.02
 C3A-C4A \\sim C3B-C4B
 with sigma of 0.02
 C5A-C4A \\sim C5B-C4B
 with sigma of 0.02
 C5A-C6A \\sim C5B-C6B
 with sigma of 0.02
 C6A-C7 \\sim C7-C6B
 with sigma of 0.02
 S2-O9 \\sim S7-O9
 with sigma of 0.02
 O10B-C30 \\sim O11A-C30
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C3B \\sim C4B \\sim C5B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
S1A \\sim S1B \\sim O10A \\sim O10B \\sim O11A \\sim O11B \\sim N4 \\sim N5A
\\sim N5B \\sim N6A \\sim N6B \\sim N29 \\sim C3A \\sim C3B \\sim C4A \\sim C4B
\\sim C5A \\sim C5B \\sim C6A \\sim C6B \\sim C21A \\sim C21B \\sim C22A \\sim
C22B \\sim C23A \\sim C23B \\sim C24A \\sim C24B \\sim C25A \\sim C25B \\sim
C27A \\sim C27B \\sim C28A \\sim C28B \\sim C29A \\sim C29B \\sim C30: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
S2 \\sim S7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N6B) = Uanis(N6A)
5. Rigid body (RIGU) restrains
 S1A, S1B, O10A, O10B, O11A, O11B, N4, N5A, N5B, N6A, N6B, N29, C3A, C3B, C4A,
 C4B, C5A, C5B, C6A, C6B, C21A, C21B, C22A, C22B, C23A, C23B, C24A, C24B, C25A,
 C25B, C27A, C27B, C28A, C28B, C29A, C29B, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S2, S7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(S1B)=Sof(O10B)=Sof(O11B)=Sof(N5B)=Sof(H5B)=Sof(N6B)=Sof(H6B)=Sof(N29)=
 Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5BA)=Sof(C6B)=Sof(H7BC)=
 Sof(H7BD)=Sof(H20C)=Sof(H20D)=Sof(C21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=
 Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(C27B)=Sof(C28B)=Sof(H28A)=Sof(H28B)=
 Sof(C29B)=Sof(H29A)=Sof(H29B)=1-FVAR(1)
 Sof(S1A)=Sof(O10A)=Sof(O11A)=Sof(N4)=Sof(N5A)=Sof(H5A)=Sof(N6A)=Sof(H6A)=
 Sof(C6A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H7AA)=
 Sof(H7AB)=Sof(H20A)=Sof(H20B)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=
 Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(C27A)=Sof(C28A)=Sof(H28C)=Sof(H28D)=
 Sof(C29A)=Sof(H29C)=Sof(H29D)=FVAR(1)
 Sof(S7)=Sof(H31D)=Sof(H31F)=Sof(H31E)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(2)
 Sof(S2)=Sof(H31B)=Sof(H31A)=Sof(H31C)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C7(H7AA,H7AB), C7(H7BC,H7BD), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
  C16(H16A,H16B), C17(H17A,H17B), C19(H19A,H19B), C20(H20A,H20B), C20(H20C,
 H20D), C28A(H28C,H28D), C28B(H28A,H28B), C29A(H29C,H29D), C29B(H29A,H29B)
7.b Me refined with riding coordinates:
 C31(H31A,H31B,H31C), C31(H31D,H31E,H31F), C32(H32A,H32B,H32C), C32(H32D,H32E,
 H32F)
7.c Aromatic/amide H refined with riding coordinates:
 N5A(H5A), N5B(H5B), N6A(H6A), N6B(H6B), C3B(H3B), C4B(H4B), C5B(H5BA),
 C3A(H3A), C4A(H4A), C5A(H5AA), C22A(H22A), C22B(H22B), C24A(H24A), C24B(H24B)
7.d Fitted hexagon refined as free rotating group:
 C6A(N1,C2,C3A,C4A,C5A)
;
_shelx_res_checksum              47723
_shelx_hkl_checksum              42925
_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 1.627
_oxdiff_exptl_absorpt_empirical_full_min 0.673