#------------------------------------------------------------------------------
#$Date: 2023-11-06 09:06:31 +0200 (Mon, 06 Nov 2023) $
#$Revision: 287325 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/98/1569871.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_1569871
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         'C45 H62 B O P'
_chemical_formula_sum            'C45 H62 B O P'
_chemical_formula_weight         660.791
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-12 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.371(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3698(1)
_cell_length_b                   42.8233(3)
_cell_length_c                   10.2352(1)
_cell_measurement_reflns_used    37303
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      79.5360
_cell_measurement_theta_min      4.1030
_cell_volume                     3995.51(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9918
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  14.18   0.38    1.10    --  -49.70  72.00 111.00  211
  2  ω   -112.00 -33.72   0.38    1.10    --  -49.70 -72.00 -18.00  206
  3  ω      2.00  46.08   0.38    1.10    --   49.70 -72.00 -18.00  116
  4  ω     52.00  77.08   0.38    1.10    --   49.70  72.00 111.00   66
  5  ω    -79.00 -53.92   0.38    4.40    --  -90.00  72.00 111.00   66
  6  ω   -141.00-115.92   0.38    4.40    --  -90.00 -72.00 -18.00   66
  7  ω    135.00 165.02   0.38    4.40    --  111.50  72.00 111.00   79
  8  ω     45.00  71.22   0.38    4.40    --  111.50 -72.00 -18.00   69
  9  ω   -119.00 -81.00   0.38    1.10    --  -49.70-125.00 150.00  100
 10  ω    -21.00   9.02   0.38    1.10    --   49.70 -19.00-180.00   79
 11  ω     -7.00  24.16   0.38    1.10    --   49.70 -19.00  90.00   82
 12  ω    -45.00 -18.78   0.38    4.40    --  -90.00  45.00 -60.00   69
 13  ω     43.00  68.08   0.38    4.40    --  111.50 -61.00  30.00   66
 14  ω     47.00  84.24   0.38    4.40    --  111.50 -76.00 156.11   98
 15  ω    120.00 153.82   0.38    4.40    --  111.50  30.00  60.00   89
 16  ω    146.00 172.22   0.38    4.40    --  111.50  30.00-120.00   69
 17  ω     43.00  69.22   0.38    4.40    --  111.50 -61.00   0.00   69
 18  ω     50.00 104.72   0.38    4.40    --  111.50 -94.00 -30.00  144
 19  ω    111.00 138.36   0.38    4.40    --  111.50  30.00-150.00   72
 20  ω     42.00  71.64   0.38    4.40    --  111.50 -94.00 120.00   78
 21  ω     69.00 116.88   0.38    4.40    --  111.50   0.00-180.00  126
 22  ω     41.00  72.92   0.38    4.40    --  111.50 -77.00 -90.00   84
 23  ω     98.00 131.06   0.38    4.40    --  111.50 125.00-180.00   87
 24  ω    119.00 145.22   0.38    4.40    --  111.50  30.00-120.00   69
 25  ω     74.00 100.22   0.38    4.40    --  111.50 -94.00 -60.00   69
 26  ω    137.00 165.88   0.38    4.40    --  111.50 125.00-180.00   76
 27  ω    129.00 155.22   0.38    4.40    --  111.50  77.00 120.00   69
 28  ω     63.00 110.12   0.38    4.40    --  111.50-125.00  90.00  124
 29  ω    114.00 149.34   0.38    4.40    --  111.50  61.00-120.00   93
 30  ω    134.00 169.72   0.38    4.40    --  111.50  61.00 150.00   94
 31  ω     98.00 177.04   0.38    4.40    --  111.50 125.00 -60.00  208
 32  ω     95.00 135.66   0.38    4.40    --  111.50 125.00 150.00  107
 33  ω    152.00 177.08   0.38    4.40    --  111.50 125.00 150.00   66
 34  ω    100.00 127.36   0.38    4.40    --  111.50  77.00  60.00   72
 35  ω    104.00 149.22   0.38    4.40    --  111.50  45.00  60.00  119
 36  ω     99.00 137.00   0.38    4.40    --  111.50  61.00  90.00  100
 37  ω    152.00 177.08   0.38    4.40    --  111.50  61.00  90.00   66
 38  ω     42.00  70.12   0.38    4.40    --  111.50 -61.00 -60.00   74
 39  ω     44.00  81.24   0.38    4.40    --  111.50 -77.00-150.00   98
 40  ω     41.00  67.22   0.38    4.40    --  111.50 -94.00 -60.00   69
 41  ω     78.00 108.78   0.38    4.40    --  111.50 -79.00 -52.90   81
 42  ω    147.00 172.08   0.38    4.40    --  111.50  30.00 -90.00   66
 43  ω    139.00 174.34   0.38    4.40    --  111.50  45.00  30.00   93
 44  ω    130.00 156.22   0.38    4.40    --  111.50  45.00  90.00   69
 45  ω     96.00 129.06   0.38    4.40    --  111.50  77.00  30.00   87
 46  ω    145.00 170.08   0.38    4.40    --  111.50  77.00  30.00   66
 47  ω     42.00  68.22   0.38    4.40    --  111.50 -61.00-120.00   69
 48  ω     42.00  84.18   0.38    4.40    --  111.50 -77.00 120.00  111
 49  ω     43.00  70.36   0.38    4.40    --  111.50 -94.00-120.00   72
 50  ω     54.00  84.78   0.38    4.40    --  111.50-125.00 120.00   81
 51  ω    112.00 137.08   0.38    4.40    --  111.50  45.00-180.00   66
 52  ω    121.00 149.12   0.38    4.40    --  111.50  45.00-150.00   74
 53  ω     99.00 132.06   0.38    4.40    --  111.50 125.00  60.00   87
 54  ω     64.00 113.02   0.38    4.40    --  111.50   0.00  90.00  129
 55  ω    -61.00   5.12   0.38    1.10    --  -49.70  77.00 -30.00  174
 56  ω   -118.00 -92.92   0.38    1.10    --  -49.70 -77.00  30.00   66
 57  ω    -73.00 -31.96   0.38    1.10    --  -49.70 -77.00  60.00  108
 58  ω    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00-150.00   72
 59  ω    -98.00 -46.70   0.38    1.10    --  -49.70 -23.00  90.65  135
 60  ω    -71.00 -38.70   0.38    1.10    --  -49.70 -57.00-150.00   85
 61  ω    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00 150.00   72
 62  ω    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00-180.00   72
 63  ω    -65.00 -38.78   0.38    1.10    --  -49.70 -57.00  60.00   69
 64  ω    -91.00 -44.64   0.38    1.10    --  -49.70   0.00-150.00  122
 65  ω    -64.00 -30.94   0.38    1.10    --  -49.70 -77.00  30.00   87
 66  ω    -86.00 -58.64   0.38    1.10    --  -49.70 125.00  90.00   72
 67  ω    -68.00 -30.76   0.38    1.10    --  -49.70 -77.00 120.00   98
 68  ω    -98.00 -44.80   0.38    1.10    --  -49.70 -37.00 120.00  140
 69  ω    -89.00 -46.82   0.38    1.10    --  -49.70 -19.00 150.00  111
 70  ω    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00 -30.00   72
 71  ω    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00 -90.00   72
 72  ω    -57.00 -30.78   0.38    1.10    --  -49.70 -77.00 -60.00   69
 73  ω    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00  90.00   72
 74  ω    -76.00 -40.66   0.38    1.10    --  -49.70 -52.00 114.08   93
 75  ω    -60.00 -30.74   0.38    1.10    --  -49.70 -77.00-120.00   77
 76  ω     57.00 107.16   0.38    1.10    --   49.70  19.00 -30.00  132
 77  ω     45.00  78.06   0.38    1.10    --   49.70  37.00   0.00   87
 78  ω     43.00  71.12   0.38    1.10    --   49.70  57.00-120.00   74
 79  ω     44.00  89.22   0.38    1.10    --   49.70  37.00-180.00  119
 80  ω     39.00  64.08   0.38    1.10    --   49.70  57.00-150.00   66
 81  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00 -14.11   69
 82  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00   0.00   69
 83  ω    -99.00 -72.78   0.38    4.40    --  -90.00 -73.00-115.83   69
 84  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00  32.53   69
 85  ω    -99.00 -71.64   0.38    4.40    --  -90.00 -75.00   9.02   72
 86  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00-170.91   69
 87  ω   -160.00-134.92   0.38    4.40    --  -90.00 -77.00 160.73   66
 88  ω   -100.00 -73.78   0.38    4.40    --  -90.00 -71.00 104.69   69
 89  ω   -160.00-133.78   0.38    4.40    --  -90.00 -75.00 103.97   69
 90  ω    -99.00 -72.78   0.38    4.40    --  -90.00 -75.00 103.97   69
 91  ω   -101.00 -74.78   0.38    4.40    --  -90.00 -74.00 169.01   69
 92  ω   -100.00 -73.78   0.38    4.40    --  -90.00 -70.00 -58.44   69
 93  ω    -96.00 -70.92   0.38    4.40    --  -90.00 -77.00 160.73   66
 94  ω    -98.00 -72.92   0.38    4.40    --  -90.00 -73.00  56.30   66
 95  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00 -40.47   69
 96  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00-175.32   69
 97  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 -77.46   69
 98  ω    -99.00 -72.78   0.38    4.40    --  -90.00 -72.00-139.45   69
 99  ω   -105.00 -77.64   0.38    4.40    --  -90.00 -61.00  30.00   72
100  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 -26.75   69
101  ω   -100.00 -72.64   0.38    4.40    --  -90.00 -73.00  13.94   72
102  ω   -102.00 -74.64   0.38    4.40    --  -90.00 -69.00 119.56   72
103  ω   -148.00-121.78   0.38    4.40    --  -90.00 -76.00  68.32   69
104  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -75.00-144.08   69
105  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 133.91   69
106  ω    -98.00 -70.64   0.38    4.40    --  -90.00 -77.00 -60.00   72
107  ω   -104.00 -77.78   0.38    4.40    --  -90.00 -61.00  60.00   69
108  ω    -97.00 -71.92   0.38    4.40    --  -90.00 -76.00  68.32   66
109  ω   -142.00-115.78   0.38    4.40    --  -90.00 -73.00  56.30   69
110  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 150.00   69
111  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00  90.00   69
112  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -75.00-101.01   69
113  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00-156.08   69
114  ω    -98.00 -71.78   0.38    4.40    --  -90.00 -75.00-125.59   69
115  ω    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 -90.00   69
116  ω   -101.00 -73.64   0.38    4.40    --  -90.00 -71.00-168.04   72
117  ω     93.00 133.28   0.38    4.40    --  111.50  77.00   0.00  106
118  ω    142.00 174.30   0.38    4.40    --  111.50  77.00-180.00   85
119  ω    140.00 167.36   0.38    4.40    --  111.50  72.00 146.96   72
120  ω     92.00 119.36   0.38    4.40    --  111.50  77.00-180.00   72
121  ω     93.00 119.22   0.38    4.40    --  111.50  77.00  60.00   69
122  ω    100.00 142.18   0.38    4.40    --  111.50  61.00 -30.00  111
123  ω     95.00 123.12   0.38    4.40    --  111.50  72.00 146.96   74
124  ω    146.00 176.02   0.38    4.40    --  111.50  45.00 -60.00   79
125  ω    117.00 143.22   0.38    4.40    --  111.50  45.00 -60.00   69
126  ω    142.00 174.30   0.38    4.40    --  111.50  60.00 -53.81   85
127  ω    151.00 177.22   0.38    4.40    --  111.50 125.00  30.00   69
128  ω     99.00 134.34   0.38    4.40    --  111.50  60.00 -53.81   93
129  ω     95.00 142.88   0.38    4.40    --  111.50 125.00  30.00  126
130  ω     99.00 125.22   0.38    4.40    --  111.50  61.00-150.00   69
131  ω     98.00 165.64   0.38    4.40    --  111.50  61.00 120.00  178
132  ω     50.00  76.22   0.38    4.40    --  111.50-125.00   0.00   69
133  ω    138.00 164.22   0.38    4.40    --  111.50  77.00  30.00   69
134  ω     92.00 117.08   0.38    4.40    --  111.50  77.00  30.00   66
135  ω     92.00 119.36   0.38    4.40    --  111.50  77.00 -30.00   72
136  ω    152.00 177.08   0.38    4.40    --  111.50  77.00 120.00   66
137  ω     92.00 126.20   0.38    4.40    --  111.50  77.00 120.00   90
138  ω    106.00 132.22   0.38    4.40    --  111.50 -81.00 138.47   69
139  ω     98.00 155.00   0.38    4.40    --  111.50  61.00 -90.00  150
140  ω     94.00 120.22   0.38    4.40    --  111.50  77.00 -60.00   69
141  ω     59.00  85.22   0.38    4.40    --  111.50 -81.00 138.47   69
142  ω     91.00 133.18   0.38    4.40    --  111.50 -83.00  12.66  111
143  ω     45.00  84.14   0.38    4.40    --  111.50-125.00 -60.00  103
144  ω     41.00  91.16   0.38    4.40    --  111.50-125.00-120.00  132
145  ω     42.00  72.78   0.38    4.40    --  111.50 -83.00  12.66   81
146  ω    142.00 172.02   0.38    4.40    --  111.50  61.00-180.00   79
147  ω     79.00 105.22   0.38    4.40    --  111.50 -97.00  59.73   69
148  ω     98.00 133.72   0.38    4.40    --  111.50  61.00-180.00   94
149  ω     41.00  67.22   0.38    4.40    --  111.50 -97.00  59.73   69
150  ω    133.00 159.22   0.38    4.40    --  111.50  61.00-120.00   69
151  ω     98.00 124.22   0.38    4.40    --  111.50  61.00-120.00   69
152  ω     96.00 122.22   0.38    4.40    --  111.50 -87.00 -18.77   69
153  ω    141.00 171.02   0.38    4.40    --  111.50  77.00 150.00   79
154  ω     92.00 129.24   0.38    4.40    --  111.50  77.00 150.00   98
155  ω     41.00  70.64   0.38    4.40    --  111.50 -87.00 -18.77   78
156  ω    129.00 176.12   0.38    4.40    --  111.50  77.00 -30.00  124
157  ω     99.00 148.02   0.38    4.40    --  111.50  61.00  30.00  129
158  ω    139.00 165.22   0.38    4.40    --  111.50  67.00-100.92   69
159  ω    139.00 172.82   0.38    4.40    --  111.50  77.00-150.00   89
160  ω     82.00 109.36   0.38    4.40    --  111.50-125.00   0.00   72
161  ω     92.00 119.36   0.38    4.40    --  111.50  77.00-150.00   72
162  ω    136.00 171.34   0.38    4.40    --  111.50  61.00-150.00   93
163  ω     96.00 136.28   0.38    4.40    --  111.50  67.00-100.92  106
164  ω    106.00 131.08   0.38    4.40    --  111.50 -88.00 -43.68   66
165  ω     80.00 106.22   0.38    4.40    --  111.50-125.00 -30.00   69
166  ω     41.00  68.36   0.38    4.40    --  111.50 -88.00 -43.68   72
167  ω     50.00  75.08   0.38    4.40    --  111.50-125.00 -30.00   66
168  ω     76.00 107.92   0.38    4.40    --  111.50-115.00-179.11   84
169  ω     55.00 105.16   0.38    4.40    --  111.50 -94.00  90.00  132
170  ω     92.00 127.34   0.38    4.40    --  111.50  77.00  90.00   93
171  ω     69.00 104.72   0.38    4.40    --  111.50 -94.00-150.00   94
172  ω    142.00 175.06   0.38    4.40    --  111.50  77.00 -90.00   87
173  ω     42.00  71.64   0.38    4.40    --  111.50-115.00-179.11   78
174  ω    149.00 177.12   0.38    4.40    --  111.50  77.00  60.00   74
175  ω     92.00 130.76   0.38    4.40    --  111.50  77.00 -90.00  102
176  ω     72.00 105.06   0.38    4.40    --  111.50 -94.00-180.00   87
177  ω     41.00  66.08   0.38    4.40    --  111.50 -61.00 150.00   66
178  ω    141.00 173.30   0.38    4.40    --  111.50  60.00-140.98   85
179  ω     98.00 124.22   0.38    4.40    --  111.50  61.00 150.00   69
180  ω     99.00 146.12   0.38    4.40    --  111.50  61.00  60.00  124
181  ω    100.00 126.22   0.38    4.40    --  111.50  60.00-140.98   69
182  ω     75.00 106.92   0.38    4.40    --  111.50-106.00-101.10   84
183  ω    135.00 177.18   0.38    4.40    --  111.50  30.00 150.00  111
184  ω    144.00 171.36   0.38    4.40    --  111.50  30.00  90.00   72
185  ω     65.00 105.66   0.38    4.40    --  111.50-125.00-180.00  107
186  ω    112.00 138.22   0.38    4.40    --  111.50  30.00  90.00   69
187  ω    150.00 176.22   0.38    4.40    --  111.50  63.00  -7.00   69
188  ω     43.00  69.22   0.38    4.40    --  111.50 -77.00  90.00   69
189  ω     98.00 124.22   0.38    4.40    --  111.50  61.00  90.00   69
190  ω     98.00 125.36   0.38    4.40    --  111.50  61.00 -60.00   72
191  ω    126.00 177.30   0.38    4.40    --  111.50  77.00-120.00  135
192  ω     41.00  67.22   0.38    4.40    --  111.50 -94.00-180.00   69
193  ω    150.00 176.22   0.38    4.40    --  111.50  61.00   0.00   69
194  ω     43.00  68.08   0.38    4.40    --  111.50 -94.00 -90.00   66
195  ω     71.00 105.20   0.38    4.40    --  111.50 -94.00 -90.00   90
196  ω     79.00 105.22   0.38    4.40    --  111.50 -94.00 150.00   69
197  ω    108.00 133.08   0.38    4.40    --  111.50  61.00   0.00   66
198  ω     93.00 120.36   0.38    4.40    --  111.50  77.00-120.00   72
199  ω     98.00 141.70   0.38    4.40    --  111.50  63.00  -7.00  115
200  ω     42.00  71.26   0.38    4.40    --  111.50-106.00-101.10   77
;
_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      -0.1150841000
_diffrn_orient_matrix_UB_12      0.0199401000
_diffrn_orient_matrix_UB_13      -0.0963911000
_diffrn_orient_matrix_UB_21      0.1231079000
_diffrn_orient_matrix_UB_22      0.0208811000
_diffrn_orient_matrix_UB_23      -0.0288087000
_diffrn_orient_matrix_UB_31      0.0128946000
_diffrn_orient_matrix_UB_32      -0.0214657000
_diffrn_orient_matrix_UB_33      -0.1174713000
_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  0.0399
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9918
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            172476
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9918
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         79.91
_diffrn_reflns_theta_min         4.13
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             1440.000
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.2899
_refine_diff_density_min         -0.1954
_refine_diff_density_rms         0.0288
_refine_ls_d_res_high            0.7830
_refine_ls_d_res_low             10.7058
_refine_ls_goodness_of_fit_ref   1.0991
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     991
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0987
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0195P)²+0.5468P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0557
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              54
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                7954
_reflns_number_total             8631
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc03433j2.cif
_cod_data_source_block           MS116V2
_cod_depositor_comments
'Adding full bibliography for 1569871--1569873.cif.'
_cod_database_code               1569871
_chemical_oxdiff_formula         'C45 H62 B O P'
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(H25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.566
_oxdiff_exptl_absorpt_empirical_full_min 0.586
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 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_refinement_flags_posn
_atom_site_refinement_flags_adp
P1 P 0.90068(2) 0.358889(4) 0.36204(2) 0.02797(5) Uani 1.000000 . .
O1 O 0.80239(5) 0.376115(12) 0.49306(5) 0.02664(11) Uani 1.000000 . .
C1 C 0.61260(8) 0.345307(16) 0.35189(7) 0.02418(14) Uani 1.000000 . .
C2 C 0.47614(9) 0.331339(18) 0.30380(8) 0.02940(16) Uani 1.000000 . .
H2 H 0.3894(11) 0.3352(2) 0.3556(11) 0.050(3) Uani 1.000000 . .
C3 C 0.45098(10) 0.312778(19) 0.18884(9) 0.03520(18) Uani 1.000000 . .
H3 H 0.3426(11) 0.3026(3) 0.1513(11) 0.057(3) Uani 1.000000 . .
C4 C 0.56236(10) 0.308401(19) 0.12109(9) 0.03562(18) Uani 1.000000 . .
H4 H 0.5423(12) 0.2948(3) 0.0271(11) 0.057(3) Uani 1.000000 . .
C5 C 0.70031(10) 0.321823(18) 0.16913(8) 0.03147(17) Uani 1.000000 . .
H5 H 0.7867(11) 0.3181(2) 0.1140(10) 0.050(3) Uani 1.000000 . .
C6 C 0.72569(8) 0.340079(16) 0.28546(7) 0.02557(15) Uani 1.000000 . .
C7 C 1.01905(10) 0.34067(2) 0.50838(10) 0.03797(19) Uani 1.000000 . .
H7a H 1.0918(15) 0.3579(3) 0.5607(14) 0.086(5) Uani 1.000000 . .
H7b H 0.9536(13) 0.3321(3) 0.5776(12) 0.064(3) Uani 1.000000 . .
H7c H 1.0837(14) 0.3222(3) 0.4779(13) 0.079(4) Uani 1.000000 . .
C8 C 1.01037(11) 0.34395(3) 0.24281(12) 0.0429(2) Uani 1.000000 . .
H8a H 1.1219(11) 0.3533(3) 0.2808(13) 0.065(4) Uani 1.000000 . .
H8b H 1.0193(12) 0.3188(3) 0.2470(13) 0.064(3) Uani 1.000000 . .
H8c H 0.9656(14) 0.3518(3) 0.1368(12) 0.065(4) Uani 1.000000 . .
C9 C 0.92411(13) 0.39981(2) 0.32352(12) 0.0421(2) Uani 1.000000 . .
H9a H 0.8201(16) 0.4125(3) 0.3139(18) 0.094(5) Uani 1.000000 . .
H9b H 1.000(2) 0.4094(3) 0.4029(17) 0.114(6) Uani 1.000000 . .
H9c H 0.9581(17) 0.4023(3) 0.2297(14) 0.088(5) Uani 1.000000 . .
C10 C 0.54761(7) 0.382670(15) 0.54944(7) 0.02136(13) Uani 1.000000 . .
C11 C 0.50750(8) 0.366660(16) 0.65572(7) 0.02255(14) Uani 1.000000 . .
C12 C 0.39114(8) 0.377783(17) 0.70720(8) 0.02705(15) Uani 1.000000 . .
H12 H 0.3618(11) 0.3657(2) 0.7902(10) 0.044(3) Uani 1.000000 . .
C13 C 0.31531(9) 0.404660(18) 0.65484(8) 0.02905(16) Uani 1.000000 . .
H13 H 0.2248(11) 0.4128(2) 0.6938(11) 0.048(3) Uani 1.000000 . .
C14 C 0.36033(8) 0.421619(17) 0.55514(8) 0.02738(15) Uani 1.000000 . .
H14 H 0.3066(11) 0.4433(2) 0.5193(11) 0.048(3) Uani 1.000000 . .
C15 C 0.47693(8) 0.411087(15) 0.50305(7) 0.02249(14) Uani 1.000000 . .
C16 C 0.59622(8) 0.339204(16) 0.72050(7) 0.02325(14) Uani 1.000000 . .
C17 C 0.53606(8) 0.308915(16) 0.71265(7) 0.02481(15) Uani 1.000000 . .
C18 C 0.62079(8) 0.284172(18) 0.77906(8) 0.02740(15) Uani 1.000000 . .
H18 H 0.5714(10) 0.2614(2) 0.7723(10) 0.047(3) Uani 1.000000 . .
C19 C 0.76366(8) 0.288524(17) 0.85247(7) 0.02665(15) Uani 1.000000 . .
C20 C 0.82266(9) 0.318626(18) 0.85784(7) 0.02716(15) Uani 1.000000 . .
H20 H 0.9341(10) 0.3221(2) 0.9150(10) 0.044(3) Uani 1.000000 . .
C21 C 0.74213(8) 0.344128(17) 0.79516(7) 0.02526(15) Uani 1.000000 . .
C22 C 0.37995(8) 0.301973(18) 0.63669(8) 0.02982(16) Uani 1.000000 . .
H22 H 0.3360(10) 0.3230(2) 0.5815(10) 0.040(2) Uani 1.000000 . .
C23 C 0.37366(12) 0.27573(2) 0.53340(11) 0.0413(2) Uani 1.000000 . .
H23a H 0.4473(14) 0.2810(3) 0.4649(13) 0.066(3) Uani 1.000000 . .
H23b H 0.4048(13) 0.2535(3) 0.5836(12) 0.070(4) Uani 1.000000 . .
H23c H 0.2637(13) 0.2729(3) 0.4744(12) 0.069(4) Uani 1.000000 . .
C24 C 0.28374(11) 0.29375(3) 0.73389(13) 0.0458(2) Uani 1.000000 . .
H24a H 0.3249(12) 0.2730(3) 0.7932(13) 0.068(4) Uani 1.000000 . .
H24b H 0.2825(13) 0.3119(3) 0.8047(13) 0.068(4) Uani 1.000000 . .
H24c H 0.1735(12) 0.2891(3) 0.6799(13) 0.076(4) Uani 1.000000 . .
C25 C 0.85748(9) 0.262082(19) 0.92543(9) 0.03339(17) Uani 1.000000 . .
H25 H 0.9508(13) 0.2718(2) 1.0107(10) 0.060(3) Uani 1.000000 . U
C26 C 0.95021(13) 0.24775(3) 0.83634(13) 0.0510(3) Uani 1.000000 . .
H26a H 0.8701(16) 0.2371(4) 0.7411(13) 0.086(5) Uani 1.000000 . .
H26b H 1.0215(14) 0.2659(3) 0.8111(19) 0.109(6) Uani 1.000000 . .
H26c H 1.0264(14) 0.2298(3) 0.8931(16) 0.095(5) Uani 1.000000 . .
C27 C 0.76934(11) 0.23690(2) 0.97687(10) 0.03750(19) Uani 1.000000 . .
H27a H 0.6996(15) 0.2471(3) 1.0391(12) 0.070(4) Uani 1.000000 . .
H27b H 0.6987(13) 0.2241(3) 0.8919(11) 0.066(4) Uani 1.000000 . .
H27c H 0.8450(13) 0.2203(3) 1.0399(11) 0.063(3) Uani 1.000000 . .
C28 C 0.80821(9) 0.376875(18) 0.81577(8) 0.03091(17) Uani 1.000000 . .
H28 H 0.7731(11) 0.3892(2) 0.7201(10) 0.045(3) Uani 1.000000 . .
C29 C 0.97613(10) 0.37733(2) 0.85302(10) 0.0386(2) Uani 1.000000 . .
H29a H 1.0207(11) 0.3680(3) 0.9522(11) 0.055(3) Uani 1.000000 . .
H29b H 1.0228(12) 0.3642(3) 0.7794(12) 0.064(3) Uani 1.000000 . .
H29c H 1.0144(12) 0.4016(3) 0.8546(12) 0.064(3) Uani 1.000000 . .
C30 C 0.74777(13) 0.39459(2) 0.92121(11) 0.0428(2) Uani 1.000000 . .
H30a H 0.6307(13) 0.3965(3) 0.8919(12) 0.064(3) Uani 1.000000 . .
H30b H 0.7739(14) 0.3829(3) 1.0165(11) 0.064(3) Uani 1.000000 . .
H30c H 0.7945(15) 0.4177(3) 0.9338(13) 0.079(4) Uani 1.000000 . .
C31 C 0.53648(8) 0.431222(15) 0.40743(7) 0.02295(14) Uani 1.000000 . .
C32 C 0.65197(8) 0.452176(16) 0.46070(7) 0.02552(15) Uani 1.000000 . .
C33 C 0.70828(9) 0.471046(17) 0.37308(8) 0.02857(16) Uani 1.000000 . .
H33 H 0.7965(10) 0.4867(2) 0.4164(10) 0.047(3) Uani 1.000000 . .
C34 C 0.65467(8) 0.469852(17) 0.23420(8) 0.02777(15) Uani 1.000000 . .
C35 C 0.54133(8) 0.449152(17) 0.18372(8) 0.02769(15) Uani 1.000000 . .
H35 H 0.4969(11) 0.4482(2) 0.0732(9) 0.046(3) Uani 1.000000 . .
C36 C 0.48088(8) 0.429879(16) 0.26758(7) 0.02452(14) Uani 1.000000 . .
C37 C 0.71494(9) 0.455475(18) 0.61104(8) 0.03081(17) Uani 1.000000 . .
H37 H 0.6687(11) 0.4376(2) 0.6634(10) 0.051(3) Uani 1.000000 . .
C38 C 0.67289(16) 0.48694(3) 0.66238(12) 0.0500(3) Uani 1.000000 . .
H38a H 0.7219(19) 0.5063(3) 0.6140(14) 0.090(5) Uani 1.000000 . .
H38b H 0.5548(17) 0.4896(3) 0.6382(14) 0.086(5) Uani 1.000000 . .
H38c H 0.7106(15) 0.4880(3) 0.7682(12) 0.070(4) Uani 1.000000 . .
C39 C 0.88126(11) 0.45104(3) 0.64815(11) 0.0427(2) Uani 1.000000 . .
H39a H 0.9134(14) 0.4281(3) 0.6133(13) 0.074(4) Uani 1.000000 . .
H39b H 0.9359(12) 0.4689(3) 0.6037(13) 0.073(4) Uani 1.000000 . .
H39c H 0.9189(12) 0.4526(3) 0.7545(11) 0.058(3) Uani 1.000000 . .
C40 C 0.71698(10) 0.490355(19) 0.13981(9) 0.03393(18) Uani 1.000000 . .
H40 H 0.6464(13) 0.4872(3) 0.0346(9) 0.058(3) Uani 1.000000 . .
C41 C 0.87224(13) 0.48035(3) 0.13591(14) 0.0466(2) Uani 1.000000 . .
H41a H 0.9445(14) 0.4825(3) 0.2373(15) 0.070(4) Uani 1.000000 . .
H41b H 0.8757(15) 0.4566(3) 0.1060(14) 0.083(4) Uani 1.000000 . .
H41c H 0.9138(15) 0.4948(3) 0.0657(14) 0.081(4) Uani 1.000000 . .
C42 C 0.71351(13) 0.52485(2) 0.17734(11) 0.0408(2) Uani 1.000000 . .
H42a H 0.6018(13) 0.5316(3) 0.1736(14) 0.071(4) Uani 1.000000 . .
H42b H 0.7848(14) 0.5289(3) 0.2806(11) 0.059(3) Uani 1.000000 . .
H42c H 0.7546(15) 0.5394(2) 0.1044(12) 0.069(4) Uani 1.000000 . .
C43 C 0.35109(8) 0.409457(18) 0.20382(8) 0.02744(15) Uani 1.000000 . .
H43 H 0.3369(10) 0.3921(2) 0.2788(9) 0.042(2) Uani 1.000000 . .
C44 C 0.21169(10) 0.42949(2) 0.16854(10) 0.03552(18) Uani 1.000000 . .
H44a H 0.1876(11) 0.4394(3) 0.2580(12) 0.058(3) Uani 1.000000 . .
H44b H 0.2258(12) 0.4486(3) 0.0995(12) 0.062(3) Uani 1.000000 . .
H44c H 0.1167(11) 0.4159(3) 0.1176(11) 0.060(3) Uani 1.000000 . .
C45 C 0.37254(11) 0.39208(2) 0.07887(9) 0.03413(18) Uani 1.000000 . .
H45a H 0.3707(12) 0.4077(3) -0.0047(10) 0.056(3) Uani 1.000000 . .
H45b H 0.4778(13) 0.3801(3) 0.0997(11) 0.055(3) Uani 1.000000 . .
H45c H 0.2832(12) 0.3750(3) 0.0463(11) 0.057(3) Uani 1.000000 . .
B1 B 0.66230(9) 0.368607(18) 0.47303(8) 0.02222(15) Uani 1.000000 . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
B 0.00963 0.00408 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.01920 0.00962 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.05239 0.03377 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.30360 0.43703 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 7 0 0.0247
6 0 -2 0.0197
-1 28 0 0.0641
-1 -8 6 0.0716
0 -28 0 0.0296
1 3 -7 0.0504
-1 28 1 0.0685
-2 -2 7 0.0796
-6 -2 0 0.0338
-6 1 1 0.0412
-5 -6 -1 0.0392
-3 -3 6 0.0717
-2 -26 1 0.0405
1 -19 -5 0.0460
-6 -11 2 0.0450
-5 3 -2 0.0450
-6 10 0 0.0491
6 -7 -1 0.0214
6 0 1 0.0256
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
C6 P1 O1 86.67(3) . . ?
C7 P1 O1 83.72(4) . . ?
C7 P1 C6 118.57(4) . . ?
C8 P1 O1 175.16(4) . . ?
C8 P1 C6 98.17(4) . . ?
C8 P1 C7 93.88(5) . . ?
C9 P1 O1 83.34(4) . . ?
C9 P1 C6 118.12(5) . . ?
C9 P1 C7 120.65(5) . . ?
C9 P1 C8 94.34(5) . . ?
B1 O1 P1 114.45(5) . . ?
C6 C1 C2 119.62(7) . . ?
B1 C1 C2 129.01(7) . . ?
B1 C1 C6 111.31(6) . . ?
H2 C2 C1 119.5(5) . . ?
C3 C2 C1 120.32(8) . . ?
C3 C2 H2 120.1(5) . . ?
H3 C3 C2 119.2(6) . . ?
C4 C3 C2 119.80(8) . . ?
C4 C3 H3 121.0(6) . . ?
H4 C4 C3 120.6(6) . . ?
C5 C4 C3 120.57(8) . . ?
C5 C4 H4 118.8(6) . . ?
H5 C5 C4 119.3(6) . . ?
C6 C5 C4 119.44(8) . . ?
C6 C5 H5 121.2(6) . . ?
C1 C6 P1 115.08(5) . . ?
C5 C6 P1 124.70(6) . . ?
C5 C6 C1 120.21(7) . . ?
H7a C7 P1 108.4(7) . . ?
H7b C7 P1 110.4(6) . . ?
H7b C7 H7a 107.1(11) . . ?
H7c C7 P1 110.5(7) . . ?
H7c C7 H7a 108.4(11) . . ?
H7c C7 H7b 112.0(10) . . ?
H8a C8 P1 105.2(7) . . ?
H8b C8 P1 111.3(6) . . ?
H8b C8 H8a 107.0(9) . . ?
H8c C8 P1 112.8(6) . . ?
H8c C8 H8a 110.1(9) . . ?
H8c C8 H8b 110.2(9) . . ?
H9a C9 P1 110.3(7) . . ?
H9b C9 P1 108.0(7) . . ?
H9b C9 H9a 107.9(13) . . ?
H9c C9 P1 111.2(7) . . ?
H9c C9 H9a 107.9(11) . . ?
H9c C9 H9b 111.4(12) . . ?
C15 C10 C11 119.37(6) . . ?
B1 C10 C11 121.87(6) . . ?
B1 C10 C15 118.62(6) . . ?
C12 C11 C10 119.69(6) . . ?
C16 C11 C10 120.17(6) . . ?
C16 C11 C12 119.98(6) . . ?
H12 C12 C11 119.7(5) . . ?
C13 C12 C11 120.58(7) . . ?
C13 C12 H12 119.7(5) . . ?
H13 C13 C12 120.0(5) . . ?
C14 C13 C12 119.87(7) . . ?
C14 C13 H13 120.1(5) . . ?
H14 C14 C13 120.0(5) . . ?
C15 C14 C13 120.44(7) . . ?
C15 C14 H14 119.5(5) . . ?
C14 C15 C10 119.78(6) . . ?
C31 C15 C10 119.75(6) . . ?
C31 C15 C14 120.24(6) . . ?
C17 C16 C11 121.46(6) . . ?
C21 C16 C11 119.14(6) . . ?
C21 C16 C17 119.36(6) . . ?
C18 C17 C16 119.59(7) . . ?
C22 C17 C16 122.32(6) . . ?
C22 C17 C18 118.08(6) . . ?
H18 C18 C17 117.9(5) . . ?
C19 C18 C17 121.88(7) . . ?
C19 C18 H18 120.2(5) . . ?
C20 C19 C18 117.91(7) . . ?
C25 C19 C18 122.82(7) . . ?
C25 C19 C20 119.27(7) . . ?
H20 C20 C19 118.1(5) . . ?
C21 C20 C19 122.42(7) . . ?
C21 C20 H20 119.5(5) . . ?
C20 C21 C16 118.82(7) . . ?
C28 C21 C16 121.33(6) . . ?
C28 C21 C20 119.72(7) . . ?
H22 C22 C17 107.8(5) . . ?
C23 C22 C17 112.03(7) . . ?
C23 C22 H22 107.4(5) . . ?
C24 C22 C17 110.77(7) . . ?
C24 C22 H22 108.5(5) . . ?
C24 C22 C23 110.17(8) . . ?
H23a C23 C22 110.8(6) . . ?
H23b C23 C22 110.6(6) . . ?
H23b C23 H23a 109.6(10) . . ?
H23c C23 C22 110.4(6) . . ?
H23c C23 H23a 108.8(9) . . ?
H23c C23 H23b 106.6(9) . . ?
H24a C24 C22 111.2(6) . . ?
H24b C24 C22 112.1(7) . . ?
H24b C24 H24a 105.8(10) . . ?
H24c C24 C22 110.5(7) . . ?
H24c C24 H24a 108.1(9) . . ?
H24c C24 H24b 109.0(10) . . ?
H25 C25 C19 110.6(5) . . ?
C26 C25 C19 110.52(7) . . ?
C26 C25 H25 99.2(7) . . ?
C27 C25 C19 113.51(7) . . ?
C27 C25 H25 111.6(6) . . ?
C27 C25 C26 110.53(8) . . ?
H26a C26 C25 108.0(7) . . ?
H26b C26 C25 108.6(8) . . ?
H26b C26 H26a 112.9(12) . . ?
H26c C26 C25 110.5(8) . . ?
H26c C26 H26a 111.8(11) . . ?
H26c C26 H26b 105.1(10) . . ?
H27a C27 C25 111.2(6) . . ?
H27b C27 C25 110.7(6) . . ?
H27b C27 H27a 108.8(10) . . ?
H27c C27 C25 109.4(6) . . ?
H27c C27 H27a 107.7(9) . . ?
H27c C27 H27b 109.0(9) . . ?
H28 C28 C21 107.0(5) . . ?
C29 C28 C21 113.98(7) . . ?
C29 C28 H28 107.2(5) . . ?
C30 C28 C21 110.37(7) . . ?
C30 C28 H28 107.9(6) . . ?
C30 C28 C29 110.16(8) . . ?
H29a C29 C28 112.4(6) . . ?
H29b C29 C28 111.6(6) . . ?
H29b C29 H29a 108.9(9) . . ?
H29c C29 C28 109.2(6) . . ?
H29c C29 H29a 106.3(8) . . ?
H29c C29 H29b 108.1(9) . . ?
H30a C30 C28 111.3(6) . . ?
H30b C30 C28 111.4(6) . . ?
H30b C30 H30a 107.1(9) . . ?
H30c C30 C28 109.5(7) . . ?
H30c C30 H30a 108.9(10) . . ?
H30c C30 H30b 108.6(9) . . ?
C32 C31 C15 118.58(6) . . ?
C36 C31 C15 122.17(6) . . ?
C36 C31 C32 119.24(6) . . ?
C33 C32 C31 119.21(7) . . ?
C37 C32 C31 122.13(7) . . ?
C37 C32 C33 118.65(7) . . ?
H33 C33 C32 117.6(6) . . ?
C34 C33 C32 122.16(7) . . ?
C34 C33 H33 120.2(6) . . ?
C35 C34 C33 117.84(7) . . ?
C40 C34 C33 121.76(7) . . ?
C40 C34 C35 120.40(7) . . ?
H35 C35 C34 118.4(5) . . ?
C36 C35 C34 122.07(7) . . ?
C36 C35 H35 119.5(5) . . ?
C35 C36 C31 119.48(7) . . ?
C43 C36 C31 122.18(6) . . ?
C43 C36 C35 118.25(7) . . ?
H37 C37 C32 109.3(5) . . ?
C38 C37 C32 111.00(7) . . ?
C38 C37 H37 106.7(6) . . ?
C39 C37 C32 111.99(8) . . ?
C39 C37 H37 107.0(6) . . ?
C39 C37 C38 110.65(8) . . ?
H38a C38 C37 109.6(7) . . ?
H38b C38 C37 110.1(7) . . ?
H38b C38 H38a 109.0(11) . . ?
H38c C38 C37 109.6(6) . . ?
H38c C38 H38a 110.4(10) . . ?
H38c C38 H38b 108.1(10) . . ?
H39a C39 C37 111.5(7) . . ?
H39b C39 C37 111.4(6) . . ?
H39b C39 H39a 107.5(10) . . ?
H39c C39 C37 108.9(6) . . ?
H39c C39 H39a 109.4(9) . . ?
H39c C39 H39b 108.1(9) . . ?
H40 C40 C34 108.0(5) . . ?
C41 C40 C34 111.32(8) . . ?
C41 C40 H40 107.0(6) . . ?
C42 C40 C34 111.42(7) . . ?
C42 C40 H40 108.2(6) . . ?
C42 C40 C41 110.71(8) . . ?
H41a C41 C40 109.5(6) . . ?
H41b C41 C40 111.6(7) . . ?
H41b C41 H41a 107.2(11) . . ?
H41c C41 C40 110.3(7) . . ?
H41c C41 H41a 109.8(10) . . ?
H41c C41 H41b 108.3(10) . . ?
H42a C42 C40 109.0(7) . . ?
H42b C42 C40 110.1(6) . . ?
H42b C42 H42a 110.7(10) . . ?
H42c C42 C40 110.1(6) . . ?
H42c C42 H42a 108.2(9) . . ?
H42c C42 H42b 108.8(9) . . ?
H43 C43 C36 107.7(5) . . ?
C44 C43 C36 109.44(6) . . ?
C44 C43 H43 108.0(5) . . ?
C45 C43 C36 113.08(7) . . ?
C45 C43 H43 108.3(5) . . ?
C45 C43 C44 110.11(7) . . ?
H44a C44 C43 110.7(6) . . ?
H44b C44 C43 110.0(6) . . ?
H44b C44 H44a 109.3(9) . . ?
H44c C44 C43 111.7(6) . . ?
H44c C44 H44a 108.0(8) . . ?
H44c C44 H44b 107.0(9) . . ?
H45a C45 C43 112.3(6) . . ?
H45b C45 C43 110.6(6) . . ?
H45b C45 H45a 107.1(8) . . ?
H45c C45 C43 109.7(6) . . ?
H45c C45 H45a 107.3(8) . . ?
H45c C45 H45b 109.7(8) . . ?
C1 B1 O1 112.25(6) . . ?
C10 B1 O1 126.39(7) . . ?
C10 B1 C1 121.17(6) . . ?
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
P1 O1 1.9395(6) . ?
P1 C6 1.8322(8) . ?
P1 C7 1.8205(9) . ?
P1 C8 1.8802(10) . ?
P1 C9 1.8204(9) . ?
O1 B1 1.3206(9) . ?
C1 C2 1.3942(10) . ?
C1 C6 1.4030(10) . ?
C1 B1 1.5757(10) . ?
C2 H2 1.082(10) . ?
C2 C3 1.3941(11) . ?
C3 H3 1.090(10) . ?
C3 C4 1.3927(13) . ?
C4 H4 1.102(10) . ?
C4 C5 1.3961(12) . ?
C5 H5 1.100(9) . ?
C5 C6 1.3980(11) . ?
C7 H7a 1.060(12) . ?
C7 H7b 1.101(12) . ?
C7 H7c 1.085(12) . ?
C8 H8a 1.103(10) . ?
C8 H8b 1.080(12) . ?
C8 H8c 1.120(11) . ?
C9 H9a 1.101(13) . ?
C9 H9b 1.036(15) . ?
C9 H9c 1.085(13) . ?
C10 C11 1.4084(10) . ?
C10 C15 1.4140(9) . ?
C10 B1 1.5868(10) . ?
C11 C12 1.3996(10) . ?
C11 C16 1.5027(9) . ?
C12 H12 1.083(9) . ?
C12 C13 1.3930(11) . ?
C13 H13 1.075(9) . ?
C13 C14 1.3949(11) . ?
C14 H14 1.078(9) . ?
C14 C15 1.3967(10) . ?
C15 C31 1.5050(9) . ?
C16 C17 1.4091(10) . ?
C16 C21 1.4193(10) . ?
C17 C18 1.4019(10) . ?
C17 C22 1.5187(10) . ?
C18 H18 1.076(9) . ?
C18 C19 1.3878(10) . ?
C19 C20 1.3987(10) . ?
C19 C25 1.5196(10) . ?
C20 H20 1.083(9) . ?
C20 C21 1.3963(10) . ?
C21 C28 1.5277(10) . ?
C22 H22 1.093(9) . ?
C22 C23 1.5347(13) . ?
C22 C24 1.5302(13) . ?
C23 H23a 1.114(13) . ?
C23 H23b 1.090(11) . ?
C23 H23c 1.074(11) . ?
C24 H24a 1.094(11) . ?
C24 H24b 1.063(14) . ?
C24 H24c 1.072(12) . ?
C25 H25 1.161(9) . ?
C25 C26 1.5262(14) . ?
C25 C27 1.5242(12) . ?
C26 H26a 1.177(13) . ?
C26 H26b 1.093(12) . ?
C26 H26c 1.117(11) . ?
C27 H27a 1.102(11) . ?
C27 H27b 1.109(10) . ?
C27 H27c 1.101(10) . ?
C28 H28 1.095(9) . ?
C28 C29 1.5310(12) . ?
C28 C30 1.5309(13) . ?
C29 H29a 1.080(11) . ?
C29 H29b 1.107(12) . ?
C29 H29c 1.098(11) . ?
C30 H30a 1.071(11) . ?
C30 H30b 1.073(12) . ?
C30 H30c 1.078(12) . ?
C31 C32 1.4144(10) . ?
C31 C36 1.4067(10) . ?
C32 C33 1.3980(10) . ?
C32 C37 1.5218(11) . ?
C33 H33 1.078(9) . ?
C33 C34 1.3947(11) . ?
C34 C35 1.3880(10) . ?
C34 C40 1.5185(10) . ?
C35 H35 1.112(9) . ?
C35 C36 1.4013(10) . ?
C36 C43 1.5174(10) . ?
C37 H37 1.080(10) . ?
C37 C38 1.5308(13) . ?
C37 C39 1.5281(13) . ?
C38 H38a 1.117(14) . ?
C38 H38b 1.082(14) . ?
C38 H38c 1.060(12) . ?
C39 H39a 1.109(12) . ?
C39 H39b 1.077(12) . ?
C39 H39c 1.066(10) . ?
C40 H40 1.134(9) . ?
C40 C41 1.5259(14) . ?
C40 C42 1.5284(12) . ?
C41 H41a 1.104(14) . ?
C41 H41b 1.063(12) . ?
C41 H41c 1.087(12) . ?
C42 H42a 1.078(12) . ?
C42 H42b 1.125(11) . ?
C42 H42c 1.108(10) . ?
C43 H43 1.099(10) . ?
C43 C44 1.5345(12) . ?
C43 C45 1.5324(11) . ?
C44 H44a 1.080(11) . ?
C44 H44b 1.108(11) . ?
C44 H44c 1.090(10) . ?
C45 H45a 1.083(11) . ?
C45 H45b 1.088(11) . ?
C45 H45c 1.103(10) . ?
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
P1 O1 B1 C1 4.05(5) . . . . ?
P1 O1 B1 C10 -170.87(4) . . . . ?
P1 C6 C1 C2 -178.28(5) . . . . ?
P1 C6 C1 B1 4.15(6) . . . . ?
P1 C6 C5 C4 179.32(7) . . . . ?
O1 B1 C1 C2 177.40(6) . . . . ?
O1 B1 C1 C6 -5.32(7) . . . . ?
O1 B1 C10 C11 -99.99(8) . . . . ?
O1 B1 C10 C15 84.31(8) . . . . ?
C1 C2 C3 C4 -0.56(9) . . . . ?
C1 C6 C5 C4 -1.14(8) . . . . ?
C1 B1 C10 C11 85.51(7) . . . . ?
C1 B1 C10 C15 -90.19(7) . . . . ?
C2 C3 C4 C5 1.57(10) . . . . ?
C3 C4 C5 C6 -0.72(10) . . . . ?
C10 C11 C12 C13 -0.43(8) . . . . ?
C10 C11 C16 C17 -115.41(7) . . . . ?
C10 C11 C16 C21 66.83(7) . . . . ?
C10 C15 C14 C13 1.48(8) . . . . ?
C10 C15 C31 C32 -84.13(7) . . . . ?
C10 C15 C31 C36 96.00(7) . . . . ?
C11 C12 C13 C14 -3.42(9) . . . . ?
C11 C16 C17 C18 -177.46(7) . . . . ?
C11 C16 C17 C22 1.17(8) . . . . ?
C11 C16 C21 C20 178.43(7) . . . . ?
C11 C16 C21 C28 2.61(8) . . . . ?
C12 C13 C14 C15 2.89(9) . . . . ?
C13 C14 C15 C31 -172.90(7) . . . . ?
C14 C15 C31 C32 90.25(7) . . . . ?
C14 C15 C31 C36 -89.62(7) . . . . ?
C15 C31 C32 C33 -179.94(6) . . . . ?
C15 C31 C32 C37 -1.44(8) . . . . ?
C15 C31 C36 C35 -179.77(7) . . . . ?
C15 C31 C36 C43 3.70(8) . . . . ?
C16 C17 C18 C19 -0.34(9) . . . . ?
C16 C17 C22 C23 126.32(8) . . . . ?
C16 C17 C22 C24 -110.22(9) . . . . ?
C16 C21 C20 C19 -1.57(8) . . . . ?
C16 C21 C28 C29 -159.53(8) . . . . ?
C16 C21 C28 C30 75.90(8) . . . . ?
C17 C18 C19 C20 -0.55(9) . . . . ?
C17 C18 C19 C25 179.91(7) . . . . ?
C18 C19 C20 C21 1.53(9) . . . . ?
C18 C19 C25 C26 93.18(9) . . . . ?
C18 C19 C25 C27 -31.66(9) . . . . ?
C19 C20 C21 C28 174.32(7) . . . . ?
C20 C21 C28 C29 24.68(8) . . . . ?
C20 C21 C28 C30 -99.89(8) . . . . ?
C31 C32 C33 C34 -0.24(8) . . . . ?
C31 C32 C37 C38 -109.62(9) . . . . ?
C31 C32 C37 C39 126.15(8) . . . . ?
C31 C36 C35 C34 -0.37(8) . . . . ?
C31 C36 C43 C44 99.67(8) . . . . ?
C31 C36 C43 C45 -137.17(8) . . . . ?
C32 C33 C34 C35 0.24(9) . . . . ?
C32 C33 C34 C40 -179.75(7) . . . . ?
C33 C34 C35 C36 0.07(9) . . . . ?
C33 C34 C40 C41 69.67(9) . . . . ?
C33 C34 C40 C42 -54.44(9) . . . . ?
C34 C35 C36 C43 176.30(7) . . . . ?
C35 C36 C43 C44 -76.90(8) . . . . ?
C35 C36 C43 C45 46.26(8) . . . . ?
loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
H25 0.0100
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
5.7699 7.2226 -0.2953 -0.4915 0.8696 -0.0459
6.0193 0.0240 -2.4344 -0.4576 0.8117 0.3631
-0.5387 27.6692 -0.0826 0.6217 0.5138 -0.5912
-1.3191 -7.5856 6.3920 -0.6156 -0.5049 -0.6051
0.4837 -27.6411 0.3187 -0.6376 -0.5268 0.5621
1.4827 2.9804 -6.6057 0.5255 0.4351 0.7311
-0.7181 27.5358 0.6216 0.5718 0.4687 -0.6734
-1.5160 -1.6739 6.6315 -0.4981 -0.4126 -0.7626
-5.8824 -2.3660 -0.0594 0.6355 -0.7719 -0.0181
-6.0556 0.9159 0.9803 0.6207 -0.7546 -0.2129
-5.3705 -6.2101 -1.3127 0.6208 -0.7530 0.2183
-3.0464 -3.4074 6.3072 -0.3253 -0.6279 -0.7071
-1.8965 -26.1995 1.2485 -0.4245 -0.8165 0.3913
1.2490 -18.8356 -4.8818 -0.0488 -0.0989 0.9939
-5.5535 -10.8410 2.1598 0.2148 -0.9723 -0.0926
-5.1331 3.2113 -2.0900 0.8562 -0.5047 0.1104
-5.5664 9.9108 0.1977 0.8192 -0.4840 -0.3077
5.8839 -6.6616 -0.9744 -0.7160 0.6133 0.3333
5.6078 -0.4807 1.0832 -0.7594 0.6491 -0.0446
