#------------------------------------------------------------------------------
#$Date: 2023-11-06 09:06:31 +0200 (Mon, 06 Nov 2023) $
#$Revision: 287325 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/98/1569872.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_1569872
loop_
_publ_author_name
'Sindlinger, Marvin'
'Ströbele, Markus'
'Grunenberg, Jörg'
'Bettinger, Holger F.'
_publ_section_title
;
 Accessing unusual heterocycles: ring expansion of benzoborirenes by
 formal cycloaddition reactions.
;
_journal_issue                   38
_journal_name_full               'Chemical science'
_journal_page_first              10478
_journal_page_last               10487
_journal_paper_doi               10.1039/d3sc03433j
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C52 H71 B N2, C7 H8'
_chemical_formula_sum            'C59 H79 B N2'
_chemical_formula_weight         827.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-16
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2022-11-16 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8427(2)
_cell_length_b                   10.73860(10)
_cell_length_c                   22.3596(2)
_cell_measurement_reflns_used    30956
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      79.5830
_cell_measurement_theta_min      3.9870
_cell_volume                     5167.04(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.70a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  -1.00   0.50    2.00    --  -49.70  80.00 112.00  138
  2  ω    -14.00  52.00   0.50    2.00    --   49.70 -80.00 -10.00  132
  3  ω    -89.00 -64.00   0.50    5.00    --  -90.00  80.00 112.00   50
  4  ω   -144.00-119.00   0.50    5.00    --  -90.00 -80.00 -10.00   50
  5  ω    101.00 171.00   0.50    5.00    --  111.50  80.00 112.00  140
  6  ω     79.00 133.00   0.50    5.00    --  111.50 -80.00 -10.00  108
  7  ω   -114.00 -73.00   0.50    2.00    --  -49.70-125.00  60.00   82
  8  ω   -118.00 -93.00   0.50    2.00    --  -49.70-125.00  90.00   50
  9  ω   -111.00 -76.00   0.50    2.00    --  -49.70-125.00  30.00   70
 10  ω    -18.00  17.00   0.50    2.00    --  -49.70  19.00-150.00   70
 11  ω    -25.00  22.00   0.50    2.00    --  -49.70  19.00-120.00   94
 12  ω    -50.00 -18.00   0.50    5.00    --  -90.00  45.00 -60.00   64
 13  ω     41.00  66.00   0.50    5.00    --  111.50 -61.00-150.00   50
 14  ω    103.00 129.00   0.50    5.00    --  111.50  61.00  90.00   52
 15  ω     42.00  70.00   0.50    5.00    --  111.50 -61.00  90.00   56
 16  ω    125.00 169.00   0.50    5.00    --  111.50 125.00 -30.00   88
 17  ω    149.00 178.00   0.50    5.00    --  111.50  61.00  90.00   58
 18  ω     41.00  77.00   0.50    5.00    --  111.50 -77.00  60.00   72
 19  ω    108.00 159.00   0.50    5.00    --  111.50  30.00 -60.00  102
 20  ω    111.00 162.00   0.50    5.00    --  111.50  61.00-120.00  102
 21  ω    109.00 135.00   0.50    5.00    --  111.50  45.00   0.00   52
 22  ω    116.00 142.00   0.50    5.00    --  111.50  61.00 150.00   52
 23  ω     76.00 114.00   0.50    5.00    --  111.50   0.00  60.00   76
 24  ω    130.00 158.00   0.50    5.00    --  111.50  77.00   0.00   56
 25  ω     44.00  70.00   0.50    5.00    --  111.50 -61.00 150.00   52
 26  ω    112.00 178.00   0.50    5.00    --  111.50  61.00-150.00  132
 27  ω     98.00 167.00   0.50    5.00    --  111.50  61.00-180.00  138
 28  ω    113.00 139.00   0.50    5.00    --  111.50  61.00  30.00   52
 29  ω     41.00  66.00   0.50    5.00    --  111.50 -61.00  30.00   50
 30  ω     98.00 127.00   0.50    5.00    --  111.50  77.00   0.00   58
 31  ω     74.00 100.00   0.50    5.00    --  111.50 -77.00   0.00   52
 32  ω    109.00 154.00   0.50    5.00    --  111.50 125.00 -90.00   90
 33  ω     62.00 106.00   0.50    5.00    --  111.50 -94.00   0.00   88
 34  ω    135.00 177.00   0.50    5.00    --  111.50  15.00-150.00   84
 35  ω    141.00 175.00   0.50    5.00    --  111.50  77.00  60.00   68
 36  ω     50.00  76.00   0.50    5.00    --  111.50 -94.00  90.00   52
 37  ω    102.00 128.00   0.50    5.00    --  111.50  77.00  60.00   52
 38  ω     41.00  95.00   0.50    5.00    --  111.50 -77.00 120.00  108
 39  ω    102.00 177.00   0.50    5.00    --  111.50  77.00 150.00  150
 40  ω     44.00  70.00   0.50    5.00    --  111.50 -60.00  53.14   52
 41  ω     72.00 126.00   0.50    5.00    --  111.50 -80.00  82.27  108
 42  ω     43.00 111.00   0.50    5.00    --  111.50-125.00  30.00  136
 43  ω    114.00 147.00   0.50    5.00    --  111.50  30.00-120.00   66
 44  ω    110.00 138.00   0.50    5.00    --  111.50  30.00  60.00   56
 45  ω    153.00 178.00   0.50    5.00    --  111.50  30.00  60.00   50
 46  ω    110.00 135.00   0.50    5.00    --  111.50  30.00  90.00   50
 47  ω    119.00 152.00   0.50    5.00    --  111.50  30.00 120.00   66
 48  ω    139.00 165.00   0.50    5.00    --  111.50  15.00  60.00   52
 49  ω     99.00 144.00   0.50    5.00    --  111.50  61.00 -30.00   90
 50  ω    142.00 168.00   0.50    5.00    --  111.50 125.00-180.00   52
 51  ω     42.00  68.00   0.50    5.00    --  111.50 -61.00   0.00   52
 52  ω    -56.00 -30.00   0.50    2.00    --  -49.70 -77.00 -60.00   52
 53  ω    -64.00 -31.00   0.50    2.00    --  -49.70 -77.00  60.00   66
 54  ω    -79.00 -44.00   0.50    2.00    --  -49.70 -37.00-180.00   70
 55  ω    -61.00 -30.00   0.50    2.00    --  -49.70 -77.00-120.00   62
 56  ω   -113.00 -49.00   0.50    2.00    --  -49.70 -25.00 104.75  128
 57  ω    -91.00 -45.00   0.50    2.00    --  -49.70 -40.00 -90.84   92
 58  ω    -56.00 -30.00   0.50    2.00    --  -49.70 -77.00   0.00   52
 59  ω    -56.00 -31.00   0.50    2.00    --  -49.70 -77.00  30.00   50
 60  ω    -69.00 -39.00   0.50    2.00    --  -49.70 -60.00 125.38   60
 61  ω   -113.00 -88.00   0.50    2.00    --  -49.70 -77.00-150.00   50
 62  ω    -84.00 -45.00   0.50    2.00    --  -49.70 -37.00   0.00   78
 63  ω    -68.00 -30.00   0.50    2.00    --  -49.70 -77.00 -90.00   76
 64  ω    -55.00 -30.00   0.50    2.00    --  -49.70 -77.00 120.00   50
 65  ω    -69.00 -41.00   0.50    2.00    --  -49.70 -55.00 -83.33   56
 66  ω    -80.00 -30.00   0.50    2.00    --  -49.70 -77.00  90.00  100
 67  ω    -64.00 -39.00   0.50    2.00    --  -49.70 -54.00 144.99   50
 68  ω    -57.00 -31.00   0.50    2.00    --  -49.70 -77.00 -30.00   52
 69  ω    -69.00 -38.00   0.50    2.00    --  -49.70 -56.00 -21.36   62
 70  ω    -57.00 -30.00   0.50    2.00    --  -49.70 -77.00 150.00   54
 71  ω   -112.00 -85.00   0.50    2.00    --  -49.70 -54.00 144.99   54
 72  ω    -58.00 -30.00   0.50    2.00    --  -49.70 -77.00-150.00   56
 73  ω    -55.00 -30.00   0.50    2.00    --  -49.70 -77.00-180.00   50
 74  ω     46.00  75.00   0.50    2.00    --   49.70  37.00   0.00   58
 75  ω     38.00  79.00   0.50    2.00    --   49.70  57.00 120.00   82
 76  ω     36.00  92.00   0.50    2.00    --   49.70-125.00   0.00  112
 77  ω      3.00  46.00   0.50    2.00    --   49.70   0.00  30.00   86
 78  ω     44.00  70.00   0.50    2.00    --   49.70  37.00  90.00   52
 79  ω    -99.00 -74.00   0.50    5.00    --  -90.00 -69.00-117.56   50
 80  ω    -98.00 -72.00   0.50    5.00    --  -90.00 -73.00  44.49   52
 81  ω   -100.00 -70.00   0.50    5.00    --  -90.00 -77.00 120.00   60
 82  ω    -98.00 -72.00   0.50    5.00    --  -90.00 -76.00 -95.56   52
 83  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00  60.00   52
 84  ω    -96.00 -71.00   0.50    5.00    --  -90.00 -75.00-176.78   50
 85  ω    -95.00 -70.00   0.50    5.00    --  -90.00 -77.00 -20.90   50
 86  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00  30.00   52
 87  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00-150.00   52
 88  ω    -97.00 -71.00   0.50    5.00    --  -90.00 -75.00 174.35   52
 89  ω    -99.00 -73.00   0.50    5.00    --  -90.00 -70.00 124.19   52
 90  ω    -98.00 -72.00   0.50    5.00    --  -90.00 -72.00 146.11   52
 91  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00-136.79   52
 92  ω   -100.00 -74.00   0.50    5.00    --  -90.00 -67.00 -54.46   52
 93  ω    -95.00 -70.00   0.50    5.00    --  -90.00 -77.00-120.00   50
 94  ω    -98.00 -73.00   0.50    5.00    --  -90.00 -71.00 135.51   50
 95  ω    -95.00 -70.00   0.50    5.00    --  -90.00 -77.00 -90.00   50
 96  ω    -99.00 -72.00   0.50    5.00    --  -90.00 -72.00  64.26   54
 97  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00  90.00   52
 98  ω   -161.00-135.00   0.50    5.00    --  -90.00 -77.00 -60.00   52
 99  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00 -60.00   52
100  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00   0.00   52
101  ω    -99.00 -73.00   0.50    5.00    --  -90.00 -71.00 -76.27   52
102  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00   6.45   52
103  ω    -96.00 -71.00   0.50    5.00    --  -90.00 -76.00 -53.62   50
104  ω    -99.00 -73.00   0.50    5.00    --  -90.00 -70.00 -20.41   52
105  ω    -98.00 -73.00   0.50    5.00    --  -90.00 -71.00  35.80   50
106  ω    -96.00 -70.00   0.50    5.00    --  -90.00 -77.00-159.18   52
107  ω    -98.00 -72.00   0.50    5.00    --  -90.00 -73.00  76.45   52
108  ω   -152.00-126.00   0.50    5.00    --  -90.00 -76.00 -53.62   52
109  ω    -97.00 -72.00   0.50    5.00    --  -90.00 -72.00 155.78   50
110  ω   -100.00 -74.00   0.50    5.00    --  -90.00 -67.00   9.07   52
111  ω   -122.00 -72.00   0.50    5.00    --  -90.00 -74.00 101.64  100
112  ω    -97.00 -71.00   0.50    5.00    --  -90.00 -76.00 -33.14   52
113  ω    133.00 159.00   0.50    5.00    --  111.50  77.00 -90.00   52
114  ω    100.00 138.00   0.50    5.00    --  111.50 125.00  90.00   76
115  ω     92.00 124.00   0.50    5.00    --  111.50  77.00 -90.00   64
116  ω    106.00 156.00   0.50    5.00    --  111.50  45.00 120.00  100
117  ω    125.00 160.00   0.50    5.00    --  111.50 125.00 120.00   70
118  ω    115.00 167.00   0.50    5.00    --  111.50  45.00  90.00  104
119  ω    146.00 171.00   0.50    5.00    --  111.50  45.00  30.00   50
120  ω    116.00 142.00   0.50    5.00    --  111.50  45.00  30.00   52
121  ω     93.00 157.00   0.50    5.00    --  111.50  77.00-120.00  128
122  ω    147.00 174.00   0.50    5.00    --  111.50  77.00-180.00   54
123  ω     45.00  70.00   0.50    5.00    --  111.50 -61.00 -90.00   50
124  ω     92.00 123.00   0.50    5.00    --  111.50  77.00-180.00   62
125  ω     58.00 108.00   0.50    5.00    --  111.50-106.00  44.34  100
126  ω    143.00 170.00   0.50    5.00    --  111.50  77.00 -60.00   54
127  ω     86.00 111.00   0.50    5.00    --  111.50-125.00-180.00   50
128  ω     92.00 129.00   0.50    5.00    --  111.50  77.00 -60.00   74
129  ω     99.00 125.00   0.50    5.00    --  111.50  61.00  60.00   52
130  ω     92.00 118.00   0.50    5.00    --  111.50  77.00   0.00   52
131  ω    133.00 176.00   0.50    5.00    --  111.50  77.00 120.00   86
132  ω     83.00 108.00   0.50    5.00    --  111.50-106.00-150.59   50
133  ω     93.00 121.00   0.50    5.00    --  111.50  77.00 120.00   56
134  ω    140.00 167.00   0.50    5.00    --  111.50  61.00   0.00   54
135  ω     48.00  74.00   0.50    5.00    --  111.50-106.00-150.59   52
136  ω    100.00 128.00   0.50    5.00    --  111.50  61.00   0.00   56
137  ω     41.00 105.00   0.50    5.00    --  111.50 -94.00 -60.00  128
138  ω     92.00 117.00   0.50    5.00    --  111.50  77.00 150.00   50
139  ω    138.00 178.00   0.50    5.00    --  111.50  77.00  30.00   80
140  ω     92.00 127.00   0.50    5.00    --  111.50  77.00  30.00   70
141  ω    117.00 166.00   0.50    5.00    --  111.50 125.00  30.00   98
142  ω    153.00 178.00   0.50    5.00    --  111.50  61.00-120.00   50
143  ω    134.00 163.00   0.50    5.00    --  111.50  15.00-180.00   58
144  ω     98.00 124.00   0.50    5.00    --  111.50  61.00 120.00   52
145  ω     46.00  91.00   0.50    5.00    --  111.50 -94.00-180.00   90
146  ω     98.00 143.00   0.50    5.00    --  111.50  61.00 -90.00   90
147  ω    101.00 127.00   0.50    5.00    --  111.50  61.00-120.00   52
148  ω    151.00 178.00   0.50    5.00    --  111.50  30.00 -30.00   54
149  ω     98.00 141.00   0.50    5.00    --  111.50  61.00 -60.00   86
150  ω    109.00 146.00   0.50    5.00    --  111.50  30.00 -30.00   74
151  ω     92.00 117.00   0.50    5.00    --  111.50  77.00  60.00   50
152  ω    137.00 163.00   0.50    5.00    --  111.50  61.00  30.00   52
153  ω     98.00 124.00   0.50    5.00    --  111.50  61.00  30.00   52
154  ω     86.00 111.00   0.50    5.00    --  111.50-125.00 -60.00   50
155  ω    151.00 177.00   0.50    5.00    --  111.50  77.00   0.00   52
156  ω     81.00 106.00   0.50    5.00    --  111.50 -94.00 150.00   50
157  ω     43.00  73.00   0.50    5.00    --  111.50-125.00-180.00   60
158  ω     42.00  68.00   0.50    5.00    --  111.50 -94.00 150.00   52
159  ω    125.00 164.00   0.50    5.00    --  111.50 125.00 150.00   78
160  ω    113.00 143.00   0.50    5.00    --  111.50  30.00-150.00   60
161  ω    148.00 174.00   0.50    5.00    --  111.50  30.00-150.00   52
162  ω     79.00 105.00   0.50    5.00    --  111.50 -94.00 -30.00   52
163  ω     41.00  72.00   0.50    5.00    --  111.50 -94.00 -30.00   62
164  ω     41.00  99.00   0.50    5.00    --  111.50 -77.00-120.00  116
165  ω     41.00  67.00   0.50    5.00    --  111.50 -60.00-157.54   52
166  ω    136.00 173.00   0.50    5.00    --  111.50  77.00  90.00   74
167  ω     80.00 105.00   0.50    5.00    --  111.50 -98.00 122.22   50
168  ω     92.00 117.00   0.50    5.00    --  111.50  77.00  90.00   50
169  ω     79.00 105.00   0.50    5.00    --  111.50 -94.00  60.00   52
170  ω     42.00  70.00   0.50    5.00    --  111.50 -98.00 122.22   56
171  ω    130.00 156.00   0.50    5.00    --  111.50  61.00 150.00   52
172  ω     98.00 124.00   0.50    5.00    --  111.50  61.00 150.00   52
173  ω     82.00 107.00   0.50    5.00    --  111.50-104.00-146.22   50
174  ω    111.00 137.00   0.50    5.00    --  111.50  30.00   0.00   52
175  ω    144.00 171.00   0.50    5.00    --  111.50 125.00  90.00   54
176  ω     93.00 118.00   0.50    5.00    --  111.50  77.00-150.00   50
177  ω    141.00 174.00   0.50    5.00    --  111.50  77.00-150.00   66
178  ω    112.00 138.00   0.50    5.00    --  111.50 125.00-120.00   52
179  ω    103.00 129.00   0.50    5.00    --  111.50  61.00-150.00   52
180  ω     42.00  76.00   0.50    5.00    --  111.50-104.00-146.22   68
181  ω     70.00 106.00   0.50    5.00    --  111.50 -94.00-120.00   72
182  ω    100.00 132.00   0.50    5.00    --  111.50 -82.00  44.89   64
183  ω    142.00 171.00   0.50    5.00    --  111.50  77.00 -30.00   58
184  ω     92.00 117.00   0.50    5.00    --  111.50  77.00 -30.00   50
185  ω    148.00 175.00   0.50    5.00    --  111.50  30.00   0.00   54
186  ω     58.00 130.00   0.50    5.00    --  111.50 -88.00-156.13  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0511035000
_diffrn_orient_matrix_UB_12      -0.0775898000
_diffrn_orient_matrix_UB_13      -0.0220794000
_diffrn_orient_matrix_UB_21      -0.0491148000
_diffrn_orient_matrix_UB_22      -0.0957815000
_diffrn_orient_matrix_UB_23      -0.0281132000
_diffrn_orient_matrix_UB_31      -0.0100968000
_diffrn_orient_matrix_UB_32      0.0733531000
_diffrn_orient_matrix_UB_33      -0.0601167000
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            211996
_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         68.243
_diffrn_reflns_theta_min         4.014
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.445
_exptl_absorpt_correction_T_max  0.94185
_exptl_absorpt_correction_T_min  0.94185
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.70a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_description       sphere
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.122
_exptl_crystal_size_rad          0.087
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         9448
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0763P)²+2.1664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8996
_reflns_number_total             9448
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc03433j2.cif
_cod_data_source_block           ms281022
_cod_depositor_comments
'Adding full bibliography for 1569871--1569873.cif.'
_cod_database_code               1569872
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C59 H79 B N2'
_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   0.948
_shelx_estimated_absorpt_t_min   0.900
_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. Restrained distances
 C54-C59 \\sim C54A-C59A
 with sigma of 0.02
 C54-C53 \\sim C54A-C53A
 with sigma of 0.02
 C59-C53 \\sim C59A-C53A
 with sigma of 0.04
 C55-C53 \\sim C55A-C53A
 with sigma of 0.04
 C54-C55 \\sim C54A-C55A
 with sigma of 0.02
 C57-C55 \\sim C57A-C55A
 with sigma of 0.04
 C58-C57 \\sim C58A-C57A
 with sigma of 0.02
 C58-C59 \\sim C58A-C59A
 with sigma of 0.02
 C54-C58 \\sim C54A-C58A
 with sigma of 0.04
 C58-C56 \\sim C58A-C56A
 with sigma of 0.04
 C54-C56 \\sim C54A-C56A
 with sigma of 0.04
 C57-C56 \\sim C57A-C56A
 with sigma of 0.02
 C59-C55 \\sim C59A-C55A
 with sigma of 0.04
 C55-C56 \\sim C55A-C56A
 with sigma of 0.02
 C57-C59 \\sim C57A-C59A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C53A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C34) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C25, C26, C32, C33, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C25A, C26, C26A, C32, C32A, C33, C33A, C34, C34A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C53, C53A, C54, C54A, C55, C55A, C56, C56A, C57, C57A, C58, C58A, C59, C59A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25A, C26A, C32A, C33A, C34A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C54A)=Sof(C55A)=Sof(H55A)=
 Sof(C56A)=Sof(H56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=
 Sof(H59A)=1-FVAR(1)
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(C55)=Sof(H55)=Sof(C56)=
 Sof(H56)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=Sof(C59)=Sof(H59)=FVAR(1)
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H27A)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(2)
 Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H27)=Sof(C32A)=Sof(H32A)=Sof(C33A)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C29(H29), C32(H32), C32A(H32A), C35(H35), C44(H44), C47(H47), C50(H50)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C19(H19), C20(H20), C21(H21), C25(H25),
 C25A(H25A), C27(H27), C27(H27A), C40(H40), C42(H42), C55(H55), C55A(H55A),
 C56(H56), C56A(H56A), C57(H57), C57A(H57A), C58(H58), C58A(H58A), C59(H59),
 C59A(H59A)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C), C33A(H33D,H33E,H33F), C34(H34A,H34B,H34C),
 C34A(H34D,H34E,H34F), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C53A(H53D,H53E,H53F)
;
_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 5.629
_oxdiff_exptl_absorpt_empirical_full_min 0.306
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.12754(5) 0.58014(10) 0.70860(5) 0.0299(2) Uani 1 1 d . . . . .
N2 N 0.15973(6) 0.40438(11) 0.82253(6) 0.0340(3) Uani 1 1 d . . . . .
C1 C 0.17623(6) 0.52466(11) 0.73584(6) 0.0263(3) Uani 1 1 d . . . . .
C2 C 0.18680(6) 0.40982(12) 0.77651(6) 0.0285(3) Uani 1 1 d . . . . .
C3 C 0.23815(6) 0.34038(12) 0.75440(6) 0.0280(3) Uani 1 1 d . . . . .
C4 C 0.27271(6) 0.42286(12) 0.72388(6) 0.0258(3) Uani 1 1 d . . . . .
C5 C 0.32109(6) 0.37557(13) 0.69702(6) 0.0325(3) Uani 1 1 d . . . . .
H5 H 0.346046 0.430492 0.678119 0.039 Uiso 1 1 calc R U . . .
C6 C 0.33267(7) 0.24901(14) 0.69791(7) 0.0398(3) Uani 1 1 d . . . . .
H6 H 0.365204 0.216993 0.679103 0.048 Uiso 1 1 calc R U . . .
C7 C 0.29689(8) 0.16848(14) 0.72622(8) 0.0441(4) Uani 1 1 d . . . . .
H7 H 0.304824 0.081509 0.726040 0.053 Uiso 1 1 calc R U . . .
C8 C 0.24982(7) 0.21309(13) 0.75471(7) 0.0392(3) Uani 1 1 d . . . . .
H8 H 0.225786 0.157396 0.774237 0.047 Uiso 1 1 calc R U . . .
C9 C 0.06323(6) 0.53431(14) 0.70540(6) 0.0344(3) Uani 1 1 d . . . . .
C10 C 0.02877(7) 0.58492(17) 0.64525(8) 0.0470(4) Uani 1 1 d . . . . .
H10A H 0.030781 0.676087 0.645662 0.071 Uiso 1 1 calc R U . . .
H10B H -0.014763 0.558316 0.639490 0.071 Uiso 1 1 calc R U . . .
H10C H 0.048140 0.552880 0.611933 0.071 Uiso 1 1 calc R U . . .
C11 C 0.03672(8) 0.58892(19) 0.75857(8) 0.0508(4) Uani 1 1 d . . . . .
H11A H 0.058210 0.552441 0.796610 0.076 Uiso 1 1 calc R U . . .
H11B H -0.007752 0.570002 0.753606 0.076 Uiso 1 1 calc R U . . .
H11C H 0.042688 0.679394 0.759631 0.076 Uiso 1 1 calc R U . . .
C12 C 0.05623(8) 0.39147(16) 0.70360(8) 0.0480(4) Uani 1 1 d . . . . .
H12A H 0.081836 0.356482 0.675771 0.072 Uiso 1 1 calc R U . . .
H12B H 0.012586 0.369624 0.689491 0.072 Uiso 1 1 calc R U . . .
H12C H 0.069829 0.357491 0.744393 0.072 Uiso 1 1 calc R U . . .
C13 C 0.17275(8) 0.31620(14) 0.87407(7) 0.0417(4) Uani 1 1 d . . . . .
C14 C 0.15034(13) 0.3848(2) 0.92644(9) 0.0719(7) Uani 1 1 d . . . . .
H14A H 0.175920 0.459093 0.937082 0.108 Uiso 1 1 calc R U . . .
H14B H 0.153946 0.329554 0.961772 0.108 Uiso 1 1 calc R U . . .
H14C H 0.106837 0.409451 0.913951 0.108 Uiso 1 1 calc R U . . .
C15 C 0.13275(9) 0.20046(17) 0.85778(10) 0.0573(5) Uani 1 1 d . . . . .
H15A H 0.088896 0.224673 0.848405 0.086 Uiso 1 1 calc R U . . .
H15B H 0.138891 0.142573 0.892171 0.086 Uiso 1 1 calc R U . . .
H15C H 0.144802 0.159838 0.822299 0.086 Uiso 1 1 calc R U . . .
C16 C 0.24082(9) 0.28333(16) 0.89409(8) 0.0500(4) Uani 1 1 d . . . . .
H16A H 0.253606 0.223681 0.865429 0.075 Uiso 1 1 calc R U . . .
H16B H 0.246674 0.246163 0.934707 0.075 Uiso 1 1 calc R U . . .
H16C H 0.266105 0.358929 0.895067 0.075 Uiso 1 1 calc R U . . .
C17 C 0.27423(6) 0.67675(11) 0.70222(5) 0.0223(2) Uani 1 1 d . . . . .
C18 C 0.32499(6) 0.71908(11) 0.74557(5) 0.0240(3) Uani 1 1 d . . . . .
C19 C 0.36168(6) 0.81772(12) 0.73210(6) 0.0271(3) Uani 1 1 d . . . . .
H19 H 0.394759 0.847274 0.761926 0.033 Uiso 1 1 calc R U . . .
C20 C 0.35003(6) 0.87292(12) 0.67524(6) 0.0283(3) Uani 1 1 d . . . . .
H20 H 0.377075 0.935583 0.664867 0.034 Uiso 1 1 calc R U . . .
C21 C 0.29880(6) 0.83623(12) 0.63367(6) 0.0271(3) Uani 1 1 d . . . . .
H21 H 0.290474 0.876003 0.595179 0.033 Uiso 1 1 calc R U . . .
C22 C 0.25897(6) 0.74208(11) 0.64692(5) 0.0234(3) Uani 1 1 d . . . . .
C23 C 0.33617(6) 0.66236(11) 0.80785(6) 0.0255(3) Uani 1 1 d . . . . .
C24 C 0.39075(6) 0.59324(12) 0.82845(6) 0.0294(3) Uani 1 1 d . . . . .
C25 C 0.3958(8) 0.5708(15) 0.8937(8) 0.038(3) Uani 0.241(8) 1 d . . P A 2
H25 H 0.433053 0.531501 0.912757 0.046 Uiso 0.241(8) 1 calc R U P A 2
C25A C 0.4004(2) 0.5358(5) 0.8849(2) 0.0287(8) Uani 0.759(8) 1 d . . P A 1
H25A H 0.436712 0.487113 0.897252 0.034 Uiso 0.759(8) 1 calc R U P A 1
C26 C 0.3542(6) 0.5987(13) 0.9307(5) 0.043(2) Uani 0.241(8) 1 d . . P A 2
C26A C 0.35691(15) 0.5494(3) 0.92353(13) 0.0293(7) Uani 0.759(8) 1 d . . P A 1
C27 C 0.30371(7) 0.62677(16) 0.90414(6) 0.0387(3) Uani 1 1 d . . . . .
H27 H 0.275458 0.641439 0.931278 0.046 Uiso 0.759(8) 1 calc R U P A 1
H27A H 0.269117 0.610852 0.923601 0.046 Uiso 0.241(8) 1 calc R U P A 2
C28 C 0.29215(6) 0.68115(12) 0.84662(6) 0.0280(3) Uani 1 1 d . . . . .
C29 C 0.44108(7) 0.57598(14) 0.78980(6) 0.0360(3) Uani 1 1 d . . . . .
H29 H 0.423031 0.599998 0.747211 0.043 Uiso 1 1 calc R U . . .
C30 C 0.46508(9) 0.44281(18) 0.78848(9) 0.0543(5) Uani 1 1 d . . . . .
H30A H 0.429824 0.385233 0.780394 0.081 Uiso 1 1 calc R U . . .
H30B H 0.490527 0.422700 0.827784 0.081 Uiso 1 1 calc R U . . .
H30C H 0.490316 0.434940 0.756418 0.081 Uiso 1 1 calc R U . . .
C31 C 0.49644(7) 0.66173(18) 0.81120(8) 0.0467(4) Uani 1 1 d . . . . .
H31A H 0.481960 0.748045 0.811654 0.070 Uiso 1 1 calc R U . . .
H31B H 0.526466 0.654526 0.783461 0.070 Uiso 1 1 calc R U . . .
H31C H 0.516351 0.637537 0.852203 0.070 Uiso 1 1 calc R U . . .
C32 C 0.3695(5) 0.5674(17) 0.9984(5) 0.065(3) Uani 0.241(8) 1 d . . P A 2
H32 H 0.332061 0.593753 1.015433 0.079 Uiso 0.241(8) 1 calc R U P A 2
C32A C 0.36753(11) 0.4940(4) 0.98681(12) 0.0448(8) Uani 0.759(8) 1 d . . P A 1
H32A H 0.326658 0.493277 1.001238 0.054 Uiso 0.759(8) 1 calc R U P A 1
C33 C 0.3748(10) 0.4373(18) 1.0094(9) 0.120(5) Uani 0.241(8) 1 d . U P A 2
H33A H 0.334782 0.397093 0.994706 0.180 Uiso 0.241(8) 1 calc R U P A 2
H33B H 0.386923 0.422279 1.053016 0.180 Uiso 0.241(8) 1 calc R U P A 2
H33C H 0.406478 0.402600 0.987887 0.180 Uiso 0.241(8) 1 calc R U P A 2
C33A C 0.39173(12) 0.3604(3) 0.98949(14) 0.0607(10) Uani 0.759(8) 1 d . . P A 1
H33D H 0.363853 0.308864 0.960574 0.091 Uiso 0.759(8) 1 calc R U P A 1
H33E H 0.393384 0.327434 1.030599 0.091 Uiso 0.759(8) 1 calc R U P A 1
H33F H 0.433493 0.359210 0.979008 0.091 Uiso 0.759(8) 1 calc R U P A 1
C34 C 0.4186(7) 0.6444(17) 1.0279(6) 0.088(4) Uani 0.241(8) 1 d . U P A 2
H34A H 0.457792 0.618826 1.015693 0.132 Uiso 0.241(8) 1 calc R U P A 2
H34B H 0.422078 0.636033 1.071946 0.132 Uiso 0.241(8) 1 calc R U P A 2
H34C H 0.409895 0.731441 1.016188 0.132 Uiso 0.241(8) 1 calc R U P A 2
C34A C 0.41184(15) 0.5758(4) 1.03039(12) 0.0590(10) Uani 0.759(8) 1 d . . P A 1
H34D H 0.452134 0.579954 1.016814 0.089 Uiso 0.759(8) 1 calc R U P A 1
H34E H 0.417370 0.540001 1.071284 0.089 Uiso 0.759(8) 1 calc R U P A 1
H34F H 0.394438 0.659773 1.031021 0.089 Uiso 0.759(8) 1 calc R U P A 1
C35 C 0.23583(7) 0.76573(12) 0.82858(6) 0.0326(3) Uani 1 1 d . . . . .
H35 H 0.220131 0.752403 0.784343 0.039 Uiso 1 1 calc R U . . .
C36 C 0.25626(10) 0.90219(14) 0.83692(9) 0.0547(5) Uani 1 1 d . . . . .
H36A H 0.220034 0.956568 0.826039 0.082 Uiso 1 1 calc R U . . .
H36B H 0.286733 0.920621 0.810677 0.082 Uiso 1 1 calc R U . . .
H36C H 0.275076 0.916570 0.879386 0.082 Uiso 1 1 calc R U . . .
C37 C 0.18206(7) 0.73952(14) 0.86238(7) 0.0392(3) Uani 1 1 d . . . . .
H37A H 0.194521 0.761043 0.905333 0.059 Uiso 1 1 calc R U . . .
H37B H 0.171181 0.650981 0.858717 0.059 Uiso 1 1 calc R U . . .
H37C H 0.145974 0.789713 0.844763 0.059 Uiso 1 1 calc R U . . .
C38 C 0.19942(6) 0.72531(11) 0.60259(5) 0.0245(3) Uani 1 1 d . . . . .
C39 C 0.18937(6) 0.62552(12) 0.56177(6) 0.0266(3) Uani 1 1 d . . . . .
C40 C 0.13565(6) 0.62400(13) 0.51767(6) 0.0301(3) Uani 1 1 d . . . . .
H40 H 0.129175 0.556359 0.489920 0.036 Uiso 1 1 calc R U . . .
C41 C 0.09141(6) 0.71799(13) 0.51301(6) 0.0313(3) Uani 1 1 d . . . . .
C42 C 0.10148(6) 0.81432(13) 0.55519(6) 0.0323(3) Uani 1 1 d . . . . .
H42 H 0.071193 0.878332 0.553382 0.039 Uiso 1 1 calc R U . . .
C43 C 0.15422(6) 0.82045(12) 0.59992(6) 0.0285(3) Uani 1 1 d . . . . .
C44 C 0.23676(6) 0.52156(13) 0.56224(6) 0.0306(3) Uani 1 1 d . . . . .
H44 H 0.269235 0.532455 0.599240 0.037 Uiso 1 1 calc R U . . .
C45 C 0.20756(8) 0.39257(14) 0.56580(8) 0.0426(4) Uani 1 1 d . . . . .
H45A H 0.176439 0.378326 0.529328 0.064 Uiso 1 1 calc R U . . .
H45B H 0.187599 0.388233 0.601799 0.064 Uiso 1 1 calc R U . . .
H45C H 0.239959 0.328690 0.568550 0.064 Uiso 1 1 calc R U . . .
C46 C 0.26881(8) 0.53047(17) 0.50683(8) 0.0478(4) Uani 1 1 d . . . . .
H46A H 0.299887 0.464162 0.508550 0.072 Uiso 1 1 calc R U . . .
H46B H 0.289252 0.611656 0.506562 0.072 Uiso 1 1 calc R U . . .
H46C H 0.237850 0.521315 0.469799 0.072 Uiso 1 1 calc R U . . .
C47 C 0.03416(7) 0.71609(14) 0.46350(7) 0.0368(3) Uani 1 1 d . . . . .
H47 H 0.038720 0.644706 0.435885 0.044 Uiso 1 1 calc R U . . .
C48 C -0.02514(8) 0.6951(2) 0.48952(8) 0.0574(5) Uani 1 1 d . . . . .
H48A H -0.022624 0.614844 0.510689 0.086 Uiso 1 1 calc R U . . .
H48B H -0.060967 0.694808 0.456457 0.086 Uiso 1 1 calc R U . . .
H48C H -0.029952 0.762045 0.518120 0.086 Uiso 1 1 calc R U . . .
C49 C 0.02883(7) 0.83458(17) 0.42560(7) 0.0445(4) Uani 1 1 d . . . . .
H49A H 0.022835 0.905998 0.451261 0.067 Uiso 1 1 calc R U . . .
H49B H -0.006720 0.827726 0.392456 0.067 Uiso 1 1 calc R U . . .
H49C H 0.066957 0.846287 0.408679 0.067 Uiso 1 1 calc R U . . .
C50 C 0.16053(7) 0.92951(13) 0.64427(7) 0.0350(3) Uani 1 1 d . . . . .
H50 H 0.200989 0.919789 0.672538 0.042 Uiso 1 1 calc R U . . .
C51 C 0.16222(9) 1.05389(15) 0.61165(9) 0.0511(4) Uani 1 1 d . . . . .
H51A H 0.123421 1.065180 0.582856 0.077 Uiso 1 1 calc R U . . .
H51B H 0.197381 1.054768 0.589686 0.077 Uiso 1 1 calc R U . . .
H51C H 0.166949 1.121638 0.641453 0.077 Uiso 1 1 calc R U . . .
C52 C 0.10853(8) 0.92704(18) 0.68270(8) 0.0500(4) Uani 1 1 d . . . . .
H52A H 0.115422 0.993766 0.713010 0.075 Uiso 1 1 calc R U . . .
H52B H 0.108730 0.846432 0.703277 0.075 Uiso 1 1 calc R U . . .
H52C H 0.068291 0.939365 0.656307 0.075 Uiso 1 1 calc R U . . .
B1 B 0.24244(7) 0.55451(13) 0.71982(6) 0.0241(3) Uani 1 1 d . . . . .
C53 C 0.4520(2) 0.8402(3) 0.94863(17) 0.0828(14) Uani 0.655(6) 1 d D . P B 1
H53A H 0.480946 0.770222 0.949575 0.124 Uiso 0.655(6) 1 calc R U P B 1
H53B H 0.411272 0.815999 0.925957 0.124 Uiso 0.655(6) 1 calc R U P B 1
H53C H 0.447839 0.862730 0.990221 0.124 Uiso 0.655(6) 1 calc R U P B 1
C53A C 0.3998(5) 0.9434(12) 0.9130(6) 0.132(4) Uani 0.345(6) 1 d D U P B 2
H53D H 0.399640 0.924786 0.955849 0.197 Uiso 0.345(6) 1 calc R U P B 2
H53E H 0.382337 0.872703 0.887993 0.197 Uiso 0.345(6) 1 calc R U P B 2
H53F H 0.374562 1.017799 0.901205 0.197 Uiso 0.345(6) 1 calc R U P B 2
C54 C 0.4757(3) 0.9471(4) 0.9190(2) 0.0566(14) Uani 0.655(6) 1 d D . P B 1
C54A C 0.4598(5) 0.9644(16) 0.9043(6) 0.084(4) Uani 0.345(6) 1 d D . P B 2
C55 C 0.4362(2) 1.0351(5) 0.8869(3) 0.0681(12) Uani 0.655(6) 1 d D . P B 1
H55 H 0.392637 1.026150 0.884805 0.082 Uiso 0.655(6) 1 calc R U P B 1
C55A C 0.4600(6) 1.0818(14) 0.8745(5) 0.099(3) Uani 0.345(6) 1 d D . P B 2
H55A H 0.423236 1.127372 0.859925 0.119 Uiso 0.345(6) 1 calc R U P B 2
C56 C 0.4583(2) 1.1347(5) 0.8581(3) 0.0705(12) Uani 0.655(6) 1 d D . P B 1
H56 H 0.430077 1.192451 0.836152 0.085 Uiso 0.655(6) 1 calc R U P B 1
C56A C 0.5155(8) 1.1211(16) 0.8690(10) 0.096(4) Uani 0.345(6) 1 d D . P B 2
H56A H 0.518245 1.200332 0.850774 0.116 Uiso 0.345(6) 1 calc R U P B 2
C57 C 0.5221(3) 1.1509(6) 0.8612(4) 0.0523(11) Uani 0.655(6) 1 d D . P B 1
H57 H 0.537621 1.220070 0.841915 0.063 Uiso 0.655(6) 1 calc R U P B 1
C57A C 0.5700(9) 1.058(3) 0.887(2) 0.074(5) Uani 0.345(6) 1 d D . P B 2
H57A H 0.607986 1.088974 0.878164 0.089 Uiso 0.345(6) 1 calc R U P B 2
C58 C 0.5614(4) 1.0672(13) 0.8917(10) 0.063(2) Uani 0.655(6) 1 d D . P B 1
H58 H 0.605075 1.078057 0.895185 0.076 Uiso 0.655(6) 1 calc R U P B 1
C58A C 0.5693(5) 0.9528(10) 0.9182(5) 0.083(3) Uani 0.345(6) 1 d D . P B 2
H58A H 0.606778 0.909367 0.932614 0.100 Uiso 0.345(6) 1 calc R U P B 2
C59 C 0.5374(3) 0.9636(4) 0.9185(2) 0.0645(11) Uani 0.655(6) 1 d D . P B 1
H59 H 0.565673 0.902182 0.937264 0.077 Uiso 0.655(6) 1 calc R U P B 1
C59A C 0.5121(6) 0.9066(14) 0.9292(5) 0.104(3) Uani 0.345(6) 1 d D . P B 2
H59A H 0.510664 0.835207 0.953974 0.125 Uiso 0.345(6) 1 calc R U P B 2
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'
B B 0.0090 0.0039 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -1 14 0.0931
-5 7 1 0.0670
3 0 -14 0.0203
9 5 -4 0.0638
3 -1 13 0.1078
7 -1 11 0.1052
-10 5 3 0.0605
-6 1 -12 0.0675
-11 -4 -1 0.1296
-7 -5 -6 0.0998
-6 -6 1 0.1349
-2 -2 -13 0.0528
-2 -7 -4 0.1174
-2 -5 -10 0.0791
2 -6 -6 0.1167
1 -1 -14 0.0208
5 -1 -14 0.0271
7 0 -14 0.0201
13 -2 -2 0.1008
12 1 -9 0.0365
13 2 -7 0.0385
14 0 -1 0.0689
13 2 0 0.0612
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
C1 N1 C9 125.02(12) . . ?
C2 N2 C13 127.20(12) . . ?
N1 C1 C2 133.53(12) . . ?
N1 C1 B1 121.08(11) . . ?
C2 C1 B1 104.36(10) . . ?
N2 C2 C1 118.36(12) . . ?
N2 C2 C3 136.13(12) . . ?
C3 C2 C1 104.51(10) . . ?
C4 C3 C2 109.83(11) . . ?
C8 C3 C2 129.36(13) . . ?
C8 C3 C4 120.40(13) . . ?
C3 C4 B1 109.92(11) . . ?
C5 C4 C3 119.06(12) . . ?
C5 C4 B1 130.53(12) . . ?
C6 C5 C4 120.08(13) . . ?
C5 C6 C7 120.20(14) . . ?
C8 C7 C6 120.96(13) . . ?
C7 C8 C3 119.21(14) . . ?
N1 C9 C10 104.21(11) . . ?
N1 C9 C11 108.58(12) . . ?
N1 C9 C12 114.94(12) . . ?
C10 C9 C11 110.76(13) . . ?
C10 C9 C12 107.45(13) . . ?
C11 C9 C12 110.71(14) . . ?
N2 C13 C14 104.10(13) . . ?
N2 C13 C15 108.00(14) . . ?
N2 C13 C16 115.19(12) . . ?
C15 C13 C14 109.19(16) . . ?
C16 C13 C14 108.12(16) . . ?
C16 C13 C15 111.85(14) . . ?
C18 C17 B1 115.19(10) . . ?
C22 C17 C18 118.66(11) . . ?
C22 C17 B1 126.06(11) . . ?
C17 C18 C23 119.22(11) . . ?
C19 C18 C17 120.54(11) . . ?
C19 C18 C23 120.10(11) . . ?
C20 C19 C18 120.13(12) . . ?
C21 C20 C19 119.63(12) . . ?
C20 C21 C22 121.63(12) . . ?
C17 C22 C38 124.42(11) . . ?
C21 C22 C17 118.89(11) . . ?
C21 C22 C38 116.48(11) . . ?
C24 C23 C18 120.64(11) . . ?
C24 C23 C28 119.94(12) . . ?
C28 C23 C18 119.40(11) . . ?
C23 C24 C25 109.1(6) . . ?
C23 C24 C29 122.02(12) . . ?
C25 C24 C29 127.4(7) . . ?
C25A C24 C23 121.2(2) . . ?
C25A C24 C29 116.7(2) . . ?
C26 C25 C24 128.6(13) . . ?
C24 C25A C26A 120.1(4) . . ?
C25 C26 C32 119.8(12) . . ?
C27 C26 C25 114.0(12) . . ?
C27 C26 C32 124.8(10) . . ?
C25A C26A C27 118.4(3) . . ?
C25A C26A C32A 121.6(3) . . ?
C27 C26A C32A 119.7(2) . . ?
C26 C27 C28 124.6(6) . . ?
C28 C27 C26A 122.03(17) . . ?
C23 C28 C35 121.62(11) . . ?
C27 C28 C23 118.05(13) . . ?
C27 C28 C35 120.19(12) . . ?
C24 C29 C30 114.16(14) . . ?
C24 C29 C31 110.99(12) . . ?
C30 C29 C31 108.33(13) . . ?
C33 C32 C26 112.6(12) . . ?
C33 C32 C34 117.3(12) . . ?
C34 C32 C26 110.4(9) . . ?
C26A C32A C33A 113.7(2) . . ?
C26A C32A C34A 110.4(3) . . ?
C33A C32A C34A 109.7(2) . . ?
C28 C35 C36 109.38(13) . . ?
C28 C35 C37 114.37(11) . . ?
C37 C35 C36 110.37(12) . . ?
C39 C38 C22 122.83(11) . . ?
C39 C38 C43 119.65(12) . . ?
C43 C38 C22 117.36(11) . . ?
C38 C39 C44 121.78(11) . . ?
C40 C39 C38 119.19(12) . . ?
C40 C39 C44 118.97(12) . . ?
C41 C40 C39 122.26(12) . . ?
C40 C41 C42 117.53(12) . . ?
C40 C41 C47 121.29(13) . . ?
C42 C41 C47 121.18(12) . . ?
C43 C42 C41 122.50(12) . . ?
C38 C43 C50 122.83(12) . . ?
C42 C43 C38 118.81(12) . . ?
C42 C43 C50 118.35(12) . . ?
C39 C44 C45 112.01(12) . . ?
C39 C44 C46 110.76(12) . . ?
C46 C44 C45 110.58(13) . . ?
C41 C47 C48 111.74(12) . . ?
C41 C47 C49 111.64(12) . . ?
C49 C47 C48 110.32(13) . . ?
C43 C50 C52 110.92(12) . . ?
C51 C50 C43 111.61(12) . . ?
C51 C50 C52 111.29(13) . . ?
C4 B1 C1 101.45(10) . . ?
C4 B1 C17 125.00(11) . . ?
C17 B1 C1 133.53(11) . . ?
C55 C54 C53 121.9(5) . . ?
C59 C54 C53 122.2(5) . . ?
C59 C54 C55 115.8(4) . . ?
C53A C54A C55A 106.9(14) . . ?
C59A C54A C53A 129.3(14) . . ?
C59A C54A C55A 122.2(11) . . ?
C56 C55 C54 122.1(4) . . ?
C56A C55A C54A 114.0(11) . . ?
C55 C56 C57 120.1(4) . . ?
C55A C56A C57A 125.6(15) . . ?
C58 C57 C56 119.2(5) . . ?
C58A C57A C56A 119.4(17) . . ?
C57 C58 C59 119.5(7) . . ?
C57A C58A C59A 118.9(12) . . ?
C54 C59 C58 123.2(5) . . ?
C54A C59A C58A 119.1(11) . . ?
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
N1 C1 1.2786(17) . ?
N1 C9 1.4784(17) . ?
N2 C2 1.2729(18) . ?
N2 C13 1.4809(18) . ?
C1 C2 1.5262(18) . ?
C1 B1 1.5812(19) . ?
C2 C3 1.4995(18) . ?
C3 C4 1.4131(18) . ?
C3 C8 1.3903(19) . ?
C4 C5 1.3975(19) . ?
C4 B1 1.5567(18) . ?
C5 C6 1.382(2) . ?
C6 C7 1.389(2) . ?
C7 C8 1.384(2) . ?
C9 C10 1.524(2) . ?
C9 C11 1.526(2) . ?
C9 C12 1.541(2) . ?
C13 C14 1.533(3) . ?
C13 C15 1.527(2) . ?
C13 C16 1.519(2) . ?
C17 C18 1.4167(17) . ?
C17 C22 1.4110(17) . ?
C17 B1 1.5665(18) . ?
C18 C19 1.3920(18) . ?
C18 C23 1.5010(17) . ?
C19 C20 1.3861(19) . ?
C20 C21 1.3838(19) . ?
C21 C22 1.3982(18) . ?
C22 C38 1.5049(17) . ?
C23 C24 1.4130(19) . ?
C23 C28 1.4150(19) . ?
C24 C25 1.464(18) . ?
C24 C25A 1.388(5) . ?
C24 C29 1.522(2) . ?
C25 C26 1.363(17) . ?
C25A C26A 1.398(4) . ?
C26 C27 1.198(13) . ?
C26 C32 1.531(15) . ?
C26A C27 1.434(4) . ?
C26A C32A 1.516(4) . ?
C27 C28 1.3955(19) . ?
C28 C35 1.5267(19) . ?
C29 C30 1.525(2) . ?
C29 C31 1.530(2) . ?
C32 C33 1.421(18) . ?
C32 C34 1.424(17) . ?
C32A C33A 1.527(4) . ?
C32A C34A 1.527(4) . ?
C35 C36 1.534(2) . ?
C35 C37 1.5280(19) . ?
C38 C39 1.4004(18) . ?
C38 C43 1.4149(18) . ?
C39 C40 1.3974(18) . ?
C39 C44 1.5212(18) . ?
C40 C41 1.389(2) . ?
C41 C42 1.392(2) . ?
C41 C47 1.5214(18) . ?
C42 C43 1.3917(19) . ?
C43 C50 1.5255(19) . ?
C44 C45 1.533(2) . ?
C44 C46 1.527(2) . ?
C47 C48 1.525(2) . ?
C47 C49 1.522(2) . ?
C50 C51 1.525(2) . ?
C50 C52 1.537(2) . ?
C53 C54 1.465(5) . ?
C53A C54A 1.376(12) . ?
C54 C55 1.392(6) . ?
C54 C59 1.361(7) . ?
C54A C55A 1.426(14) . ?
C54A C59A 1.335(12) . ?
C55 C56 1.378(5) . ?
C55A C56A 1.308(16) . ?
C56 C57 1.394(7) . ?
C56A C57A 1.373(19) . ?
C57 C58 1.345(11) . ?
C57A C58A 1.32(2) . ?
C58 C59 1.407(10) . ?
C58A C59A 1.404(12) . ?
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
-2.6293 -0.6289 14.4517 -0.4047 -0.2169 -0.8884
-4.7749 6.5639 0.9692 -0.7747 -0.4214 0.4714
3.2200 -0.2984 -14.4764 0.5073 0.2774 0.8159
9.3928 5.1408 -3.5330 0.1591 -0.8544 0.4947
3.1875 -0.8856 13.2520 -0.0610 -0.4443 -0.8938
6.6047 -0.6669 11.4164 0.1372 -0.5815 -0.8019
-9.9244 4.9235 3.2599 -0.9612 -0.0758 0.2654
-5.6057 1.3951 -11.8311 -0.1335 0.4743 0.8702
-11.0051 -4.0835 -1.4068 -0.2145 0.9712 -0.1039
-7.1136 -4.8540 -6.0939 0.1476 0.9856 0.0821
-6.2987 -6.2442 1.4156 0.1313 0.8676 -0.4795
-1.7654 -2.4876 -12.9291 0.3883 0.6885 0.6126
-2.2348 -6.5606 -3.8925 0.4808 0.8476 -0.2247
-2.1917 -4.8256 -9.6984 0.4765 0.8425 0.2512
2.1390 -6.2546 -6.3161 0.7341 0.6716 -0.1007
1.3555 -0.7664 -14.3838 0.4463 0.4112 0.7948
4.7326 -0.8207 -14.2041 0.6191 0.2455 0.7459
6.7571 0.2663 -13.7444 0.6281 0.0290 0.7776
13.2507 -2.4713 -1.9215 0.9113 -0.3601 -0.1995
11.9184 1.1443 -9.4728 0.7294 -0.4287 0.5331
13.0902 1.6193 -6.6735 0.6907 -0.6104 0.3878
14.0850 -0.0819 -0.8491 0.7449 -0.6601 -0.0972
13.4246 1.8827 0.1421 0.5368 -0.8437 -0.0060
