Accessing unusual heterocycles: ring expansion of benzoborirenes by formal cycloaddition reactions.
Sindlinger, Marvin; Ströbele, Markus; Grunenberg, Jörg; Bettinger, Holger F.; Chemical science 14 (2023) 10478–10487; doi:10.1039/d3sc03433j

data_1569871
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  14.18   0.38    1.10    --  -49.70  72.00 111.00  211
  2  \w   -112.00 -33.72   0.38    1.10    --  -49.70 -72.00 -18.00  206
  3  \w      2.00  46.08   0.38    1.10    --   49.70 -72.00 -18.00  116
  4  \w     52.00  77.08   0.38    1.10    --   49.70  72.00 111.00   66
  5  \w    -79.00 -53.92   0.38    4.40    --  -90.00  72.00 111.00   66
  6  \w   -141.00-115.92   0.38    4.40    --  -90.00 -72.00 -18.00   66
  7  \w    135.00 165.02   0.38    4.40    --  111.50  72.00 111.00   79
  8  \w     45.00  71.22   0.38    4.40    --  111.50 -72.00 -18.00   69
  9  \w   -119.00 -81.00   0.38    1.10    --  -49.70-125.00 150.00  100
 10  \w    -21.00   9.02   0.38    1.10    --   49.70 -19.00-180.00   79
 11  \w     -7.00  24.16   0.38    1.10    --   49.70 -19.00  90.00   82
 12  \w    -45.00 -18.78   0.38    4.40    --  -90.00  45.00 -60.00   69
 13  \w     43.00  68.08   0.38    4.40    --  111.50 -61.00  30.00   66
 14  \w     47.00  84.24   0.38    4.40    --  111.50 -76.00 156.11   98
 15  \w    120.00 153.82   0.38    4.40    --  111.50  30.00  60.00   89
 16  \w    146.00 172.22   0.38    4.40    --  111.50  30.00-120.00   69
 17  \w     43.00  69.22   0.38    4.40    --  111.50 -61.00   0.00   69
 18  \w     50.00 104.72   0.38    4.40    --  111.50 -94.00 -30.00  144
 19  \w    111.00 138.36   0.38    4.40    --  111.50  30.00-150.00   72
 20  \w     42.00  71.64   0.38    4.40    --  111.50 -94.00 120.00   78
 21  \w     69.00 116.88   0.38    4.40    --  111.50   0.00-180.00  126
 22  \w     41.00  72.92   0.38    4.40    --  111.50 -77.00 -90.00   84
 23  \w     98.00 131.06   0.38    4.40    --  111.50 125.00-180.00   87
 24  \w    119.00 145.22   0.38    4.40    --  111.50  30.00-120.00   69
 25  \w     74.00 100.22   0.38    4.40    --  111.50 -94.00 -60.00   69
 26  \w    137.00 165.88   0.38    4.40    --  111.50 125.00-180.00   76
 27  \w    129.00 155.22   0.38    4.40    --  111.50  77.00 120.00   69
 28  \w     63.00 110.12   0.38    4.40    --  111.50-125.00  90.00  124
 29  \w    114.00 149.34   0.38    4.40    --  111.50  61.00-120.00   93
 30  \w    134.00 169.72   0.38    4.40    --  111.50  61.00 150.00   94
 31  \w     98.00 177.04   0.38    4.40    --  111.50 125.00 -60.00  208
 32  \w     95.00 135.66   0.38    4.40    --  111.50 125.00 150.00  107
 33  \w    152.00 177.08   0.38    4.40    --  111.50 125.00 150.00   66
 34  \w    100.00 127.36   0.38    4.40    --  111.50  77.00  60.00   72
 35  \w    104.00 149.22   0.38    4.40    --  111.50  45.00  60.00  119
 36  \w     99.00 137.00   0.38    4.40    --  111.50  61.00  90.00  100
 37  \w    152.00 177.08   0.38    4.40    --  111.50  61.00  90.00   66
 38  \w     42.00  70.12   0.38    4.40    --  111.50 -61.00 -60.00   74
 39  \w     44.00  81.24   0.38    4.40    --  111.50 -77.00-150.00   98
 40  \w     41.00  67.22   0.38    4.40    --  111.50 -94.00 -60.00   69
 41  \w     78.00 108.78   0.38    4.40    --  111.50 -79.00 -52.90   81
 42  \w    147.00 172.08   0.38    4.40    --  111.50  30.00 -90.00   66
 43  \w    139.00 174.34   0.38    4.40    --  111.50  45.00  30.00   93
 44  \w    130.00 156.22   0.38    4.40    --  111.50  45.00  90.00   69
 45  \w     96.00 129.06   0.38    4.40    --  111.50  77.00  30.00   87
 46  \w    145.00 170.08   0.38    4.40    --  111.50  77.00  30.00   66
 47  \w     42.00  68.22   0.38    4.40    --  111.50 -61.00-120.00   69
 48  \w     42.00  84.18   0.38    4.40    --  111.50 -77.00 120.00  111
 49  \w     43.00  70.36   0.38    4.40    --  111.50 -94.00-120.00   72
 50  \w     54.00  84.78   0.38    4.40    --  111.50-125.00 120.00   81
 51  \w    112.00 137.08   0.38    4.40    --  111.50  45.00-180.00   66
 52  \w    121.00 149.12   0.38    4.40    --  111.50  45.00-150.00   74
 53  \w     99.00 132.06   0.38    4.40    --  111.50 125.00  60.00   87
 54  \w     64.00 113.02   0.38    4.40    --  111.50   0.00  90.00  129
 55  \w    -61.00   5.12   0.38    1.10    --  -49.70  77.00 -30.00  174
 56  \w   -118.00 -92.92   0.38    1.10    --  -49.70 -77.00  30.00   66
 57  \w    -73.00 -31.96   0.38    1.10    --  -49.70 -77.00  60.00  108
 58  \w    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00-150.00   72
 59  \w    -98.00 -46.70   0.38    1.10    --  -49.70 -23.00  90.65  135
 60  \w    -71.00 -38.70   0.38    1.10    --  -49.70 -57.00-150.00   85
 61  \w    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00 150.00   72
 62  \w    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00-180.00   72
 63  \w    -65.00 -38.78   0.38    1.10    --  -49.70 -57.00  60.00   69
 64  \w    -91.00 -44.64   0.38    1.10    --  -49.70   0.00-150.00  122
 65  \w    -64.00 -30.94   0.38    1.10    --  -49.70 -77.00  30.00   87
 66  \w    -86.00 -58.64   0.38    1.10    --  -49.70 125.00  90.00   72
 67  \w    -68.00 -30.76   0.38    1.10    --  -49.70 -77.00 120.00   98
 68  \w    -98.00 -44.80   0.38    1.10    --  -49.70 -37.00 120.00  140
 69  \w    -89.00 -46.82   0.38    1.10    --  -49.70 -19.00 150.00  111
 70  \w    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00 -30.00   72
 71  \w    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00 -90.00   72
 72  \w    -57.00 -30.78   0.38    1.10    --  -49.70 -77.00 -60.00   69
 73  \w    -58.00 -30.64   0.38    1.10    --  -49.70 -77.00  90.00   72
 74  \w    -76.00 -40.66   0.38    1.10    --  -49.70 -52.00 114.08   93
 75  \w    -60.00 -30.74   0.38    1.10    --  -49.70 -77.00-120.00   77
 76  \w     57.00 107.16   0.38    1.10    --   49.70  19.00 -30.00  132
 77  \w     45.00  78.06   0.38    1.10    --   49.70  37.00   0.00   87
 78  \w     43.00  71.12   0.38    1.10    --   49.70  57.00-120.00   74
 79  \w     44.00  89.22   0.38    1.10    --   49.70  37.00-180.00  119
 80  \w     39.00  64.08   0.38    1.10    --   49.70  57.00-150.00   66
 81  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00 -14.11   69
 82  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00   0.00   69
 83  \w    -99.00 -72.78   0.38    4.40    --  -90.00 -73.00-115.83   69
 84  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00  32.53   69
 85  \w    -99.00 -71.64   0.38    4.40    --  -90.00 -75.00   9.02   72
 86  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00-170.91   69
 87  \w   -160.00-134.92   0.38    4.40    --  -90.00 -77.00 160.73   66
 88  \w   -100.00 -73.78   0.38    4.40    --  -90.00 -71.00 104.69   69
 89  \w   -160.00-133.78   0.38    4.40    --  -90.00 -75.00 103.97   69
 90  \w    -99.00 -72.78   0.38    4.40    --  -90.00 -75.00 103.97   69
 91  \w   -101.00 -74.78   0.38    4.40    --  -90.00 -74.00 169.01   69
 92  \w   -100.00 -73.78   0.38    4.40    --  -90.00 -70.00 -58.44   69
 93  \w    -96.00 -70.92   0.38    4.40    --  -90.00 -77.00 160.73   66
 94  \w    -98.00 -72.92   0.38    4.40    --  -90.00 -73.00  56.30   66
 95  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00 -40.47   69
 96  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00-175.32   69
 97  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 -77.46   69
 98  \w    -99.00 -72.78   0.38    4.40    --  -90.00 -72.00-139.45   69
 99  \w   -105.00 -77.64   0.38    4.40    --  -90.00 -61.00  30.00   72
100  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 -26.75   69
101  \w   -100.00 -72.64   0.38    4.40    --  -90.00 -73.00  13.94   72
102  \w   -102.00 -74.64   0.38    4.40    --  -90.00 -69.00 119.56   72
103  \w   -148.00-121.78   0.38    4.40    --  -90.00 -76.00  68.32   69
104  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -75.00-144.08   69
105  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 133.91   69
106  \w    -98.00 -70.64   0.38    4.40    --  -90.00 -77.00 -60.00   72
107  \w   -104.00 -77.78   0.38    4.40    --  -90.00 -61.00  60.00   69
108  \w    -97.00 -71.92   0.38    4.40    --  -90.00 -76.00  68.32   66
109  \w   -142.00-115.78   0.38    4.40    --  -90.00 -73.00  56.30   69
110  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 150.00   69
111  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00  90.00   69
112  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -75.00-101.01   69
113  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -76.00-156.08   69
114  \w    -98.00 -71.78   0.38    4.40    --  -90.00 -75.00-125.59   69
115  \w    -97.00 -70.78   0.38    4.40    --  -90.00 -77.00 -90.00   69
116  \w   -101.00 -73.64   0.38    4.40    --  -90.00 -71.00-168.04   72
117  \w     93.00 133.28   0.38    4.40    --  111.50  77.00   0.00  106
118  \w    142.00 174.30   0.38    4.40    --  111.50  77.00-180.00   85
119  \w    140.00 167.36   0.38    4.40    --  111.50  72.00 146.96   72
120  \w     92.00 119.36   0.38    4.40    --  111.50  77.00-180.00   72
121  \w     93.00 119.22   0.38    4.40    --  111.50  77.00  60.00   69
122  \w    100.00 142.18   0.38    4.40    --  111.50  61.00 -30.00  111
123  \w     95.00 123.12   0.38    4.40    --  111.50  72.00 146.96   74
124  \w    146.00 176.02   0.38    4.40    --  111.50  45.00 -60.00   79
125  \w    117.00 143.22   0.38    4.40    --  111.50  45.00 -60.00   69
126  \w    142.00 174.30   0.38    4.40    --  111.50  60.00 -53.81   85
127  \w    151.00 177.22   0.38    4.40    --  111.50 125.00  30.00   69
128  \w     99.00 134.34   0.38    4.40    --  111.50  60.00 -53.81   93
129  \w     95.00 142.88   0.38    4.40    --  111.50 125.00  30.00  126
130  \w     99.00 125.22   0.38    4.40    --  111.50  61.00-150.00   69
131  \w     98.00 165.64   0.38    4.40    --  111.50  61.00 120.00  178
132  \w     50.00  76.22   0.38    4.40    --  111.50-125.00   0.00   69
133  \w    138.00 164.22   0.38    4.40    --  111.50  77.00  30.00   69
134  \w     92.00 117.08   0.38    4.40    --  111.50  77.00  30.00   66
135  \w     92.00 119.36   0.38    4.40    --  111.50  77.00 -30.00   72
136  \w    152.00 177.08   0.38    4.40    --  111.50  77.00 120.00   66
137  \w     92.00 126.20   0.38    4.40    --  111.50  77.00 120.00   90
138  \w    106.00 132.22   0.38    4.40    --  111.50 -81.00 138.47   69
139  \w     98.00 155.00   0.38    4.40    --  111.50  61.00 -90.00  150
140  \w     94.00 120.22   0.38    4.40    --  111.50  77.00 -60.00   69
141  \w     59.00  85.22   0.38    4.40    --  111.50 -81.00 138.47   69
142  \w     91.00 133.18   0.38    4.40    --  111.50 -83.00  12.66  111
143  \w     45.00  84.14   0.38    4.40    --  111.50-125.00 -60.00  103
144  \w     41.00  91.16   0.38    4.40    --  111.50-125.00-120.00  132
145  \w     42.00  72.78   0.38    4.40    --  111.50 -83.00  12.66   81
146  \w    142.00 172.02   0.38    4.40    --  111.50  61.00-180.00   79
147  \w     79.00 105.22   0.38    4.40    --  111.50 -97.00  59.73   69
148  \w     98.00 133.72   0.38    4.40    --  111.50  61.00-180.00   94
149  \w     41.00  67.22   0.38    4.40    --  111.50 -97.00  59.73   69
150  \w    133.00 159.22   0.38    4.40    --  111.50  61.00-120.00   69
151  \w     98.00 124.22   0.38    4.40    --  111.50  61.00-120.00   69
152  \w     96.00 122.22   0.38    4.40    --  111.50 -87.00 -18.77   69
153  \w    141.00 171.02   0.38    4.40    --  111.50  77.00 150.00   79
154  \w     92.00 129.24   0.38    4.40    --  111.50  77.00 150.00   98
155  \w     41.00  70.64   0.38    4.40    --  111.50 -87.00 -18.77   78
156  \w    129.00 176.12   0.38    4.40    --  111.50  77.00 -30.00  124
157  \w     99.00 148.02   0.38    4.40    --  111.50  61.00  30.00  129
158  \w    139.00 165.22   0.38    4.40    --  111.50  67.00-100.92   69
159  \w    139.00 172.82   0.38    4.40    --  111.50  77.00-150.00   89
160  \w     82.00 109.36   0.38    4.40    --  111.50-125.00   0.00   72
161  \w     92.00 119.36   0.38    4.40    --  111.50  77.00-150.00   72
162  \w    136.00 171.34   0.38    4.40    --  111.50  61.00-150.00   93
163  \w     96.00 136.28   0.38    4.40    --  111.50  67.00-100.92  106
164  \w    106.00 131.08   0.38    4.40    --  111.50 -88.00 -43.68   66
165  \w     80.00 106.22   0.38    4.40    --  111.50-125.00 -30.00   69
166  \w     41.00  68.36   0.38    4.40    --  111.50 -88.00 -43.68   72
167  \w     50.00  75.08   0.38    4.40    --  111.50-125.00 -30.00   66
168  \w     76.00 107.92   0.38    4.40    --  111.50-115.00-179.11   84
169  \w     55.00 105.16   0.38    4.40    --  111.50 -94.00  90.00  132
170  \w     92.00 127.34   0.38    4.40    --  111.50  77.00  90.00   93
171  \w     69.00 104.72   0.38    4.40    --  111.50 -94.00-150.00   94
172  \w    142.00 175.06   0.38    4.40    --  111.50  77.00 -90.00   87
173  \w     42.00  71.64   0.38    4.40    --  111.50-115.00-179.11   78
174  \w    149.00 177.12   0.38    4.40    --  111.50  77.00  60.00   74
175  \w     92.00 130.76   0.38    4.40    --  111.50  77.00 -90.00  102
176  \w     72.00 105.06   0.38    4.40    --  111.50 -94.00-180.00   87
177  \w     41.00  66.08   0.38    4.40    --  111.50 -61.00 150.00   66
178  \w    141.00 173.30   0.38    4.40    --  111.50  60.00-140.98   85
179  \w     98.00 124.22   0.38    4.40    --  111.50  61.00 150.00   69
180  \w     99.00 146.12   0.38    4.40    --  111.50  61.00  60.00  124
181  \w    100.00 126.22   0.38    4.40    --  111.50  60.00-140.98   69
182  \w     75.00 106.92   0.38    4.40    --  111.50-106.00-101.10   84
183  \w    135.00 177.18   0.38    4.40    --  111.50  30.00 150.00  111
184  \w    144.00 171.36   0.38    4.40    --  111.50  30.00  90.00   72
185  \w     65.00 105.66   0.38    4.40    --  111.50-125.00-180.00  107
186  \w    112.00 138.22   0.38    4.40    --  111.50  30.00  90.00   69
187  \w    150.00 176.22   0.38    4.40    --  111.50  63.00  -7.00   69
188  \w     43.00  69.22   0.38    4.40    --  111.50 -77.00  90.00   69
189  \w     98.00 124.22   0.38    4.40    --  111.50  61.00  90.00   69
190  \w     98.00 125.36   0.38    4.40    --  111.50  61.00 -60.00   72
191  \w    126.00 177.30   0.38    4.40    --  111.50  77.00-120.00  135
192  \w     41.00  67.22   0.38    4.40    --  111.50 -94.00-180.00   69
193  \w    150.00 176.22   0.38    4.40    --  111.50  61.00   0.00   69
194  \w     43.00  68.08   0.38    4.40    --  111.50 -94.00 -90.00   66
195  \w     71.00 105.20   0.38    4.40    --  111.50 -94.00 -90.00   90
196  \w     79.00 105.22   0.38    4.40    --  111.50 -94.00 150.00   69
197  \w    108.00 133.08   0.38    4.40    --  111.50  61.00   0.00   66
198  \w     93.00 120.36   0.38    4.40    --  111.50  77.00-120.00   72
199  \w     98.00 141.70   0.38    4.40    --  111.50  63.00  -7.00  115
200  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0195P)^2^+0.5468P] where P=(Fo^2^+2Fc^2^)/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