Catalyst-Controlled Regioselective Carbonylation of Isobutylene Oxide to Pivalolactone
Hubbell, Aran K.; Lamb, Jessica R.; Klimovica, Kristine; Mulzer, Michael; Shaffer, Timothy D.; MacMillan, Samantha N.; Coates, Geoffrey W.; ACS Catalysis  (2020) 12537–12543; doi:10.1021/acscatal.0c03492

data_4518134
_publ_section_title
;
 Catalyst-Controlled Regioselective Carbonylation of Isobutylene Oxide to
 Pivalolactone
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              12537
_journal_page_last               12543
_journal_paper_doi               10.1021/acscatal.0c03492
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C68 H58 Al N2 O6, C4 H8 O, C24 H20 B'
_chemical_formula_sum            'C96 H86 Al B N2 O7'
_chemical_formula_weight         1417.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-08
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.11.15 svn.r3537 for Rigaku Oxford Diffraction, GUI svn.r5585)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3470(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.16596(4)
_cell_length_b                   24.26807(8)
_cell_length_c                   21.69468(7)
_cell_measurement_reflns_used    180794
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.8150
_cell_measurement_theta_min      1.8100
_cell_volume                     7425.75(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.26a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -26.00  17.00   0.50    0.44    --  -48.30  19.00  90.00   86
  2  \w    -26.00  -1.00   0.50    0.44    --   14.00 112.00  59.07   50
  3  \w      8.00  33.00   0.50    0.44    --   38.00  95.00  52.57   50
  4  \w     26.00  51.00   0.50    0.44    --   50.00  83.00  52.23   50
  5  \w     36.00  62.00   0.50    0.44    --   58.00  77.00  81.28   52
  6  \w     73.00 100.00   0.50    0.44    --   58.00  78.00  92.89   54
  7  \w    105.00 132.00   0.50    0.44    --   70.00  77.00 118.75   54
  8  \w    128.00 154.00   0.50    1.74    --  107.75 129.00  37.00   52
  9  \w    126.00 153.00   0.50    1.74    --  107.75  77.00 -30.00   54
 10  \w    137.00 163.00   0.50    1.74    --  107.75  77.00 -60.00   52
 11  \w    150.00 178.00   0.50    1.74    --  107.75  70.00 -76.75   56
 12  \w    135.00 178.00   0.50    1.74    --  107.75  77.00 -90.00   86
 13  \w    145.00 178.00   0.50    1.74    --  107.75 125.00 -90.00   66
 14  \w    153.00 178.00   0.50    1.74    --  107.75 125.00-120.00   50
 15  \w    135.00 178.00   0.50    1.74    --  107.75  77.00-180.00   86
 16  \w    136.00 162.00   0.50    1.74    --  107.75  77.00-120.00   52
 17  \w    139.00 165.00   0.50    1.74    --  107.75  39.00-146.66   52
 18  \w    130.00 170.00   0.50    1.74    --  107.75 125.00 -60.00   80
 19  \w    140.00 174.00   0.50    1.74    --  107.75  77.00   0.00   68
 20  \w    143.00 173.00   0.50    1.74    --  107.75  77.00  70.64   60
 21  \w    143.00 169.00   0.50    1.74    --  107.75  77.00 120.00   52
 22  \w    153.00 178.00   0.50    1.74    --  107.75  77.00 150.00   50
 23  \w    135.00 172.00   0.50    1.74    --  107.75  81.00 101.54   74
 24  \w    142.00 177.00   0.50    1.74    --  107.75  45.00  60.00   70
 25  \w    145.00 171.00   0.50    1.74    --  107.75  45.00  90.00   52
 26  \w    136.00 177.00   0.50    1.74    --  107.75  61.00 120.00   82
 27  \w    137.00 170.00   0.50    1.74    --  107.75  76.00 135.48   66
 28  \w    125.00 165.00   0.50    1.74    --  107.75  77.00  30.00   80
 29  \w    139.00 175.00   0.50    1.74    --  107.75  30.00  30.00   72
 30  \w    119.00 178.00   0.50    1.74    --  107.75 125.00 150.00  118
 31  \w    119.00 177.00   0.50    1.74    --  107.75  46.00 157.26  116
 32  \w    100.00 125.00   0.50    0.44    --   54.00  80.00  26.28   50
 33  \w     91.00 117.00   0.50    0.44    --   50.00  83.00  52.23   52
 34  \w     67.00  94.00   0.50    1.74    --   90.00  81.00  64.73   54
 35  \w     82.00 110.00   0.50    1.74    --  102.00  72.00  97.35   56
 36  \w     93.00 129.00   0.50    1.74    --  107.75  61.00 120.00   72
 37  \w    101.00 127.00   0.50    1.74    --  107.75  45.00  60.00   52
 38  \w    102.00 178.00   0.50    1.74    --  107.75  42.00  47.36  152
 39  \w    104.00 169.00   0.50    1.74    --  107.75  45.00 -30.00  130
 40  \w    112.00 138.00   0.50    1.74    --  107.75 125.00-120.00   52
 41  \w    144.00 178.00   0.50    1.74    --  107.75 125.00-150.00   68
 42  \w    108.00 134.00   0.50    1.74    --  107.75 125.00-150.00   52
 43  \w    106.00 131.00   0.50    1.74    --  107.75 140.00-149.00   50
 44  \w    100.00 126.00   0.50    1.74    --  107.75 125.00 -90.00   52
 45  \w     86.00 121.00   0.50    1.74    --  107.75  77.00 -30.00   70
 46  \w     93.00 160.00   0.50    1.74    --  107.75  61.00 -90.00  134
 47  \w     93.00 166.00   0.50    1.74    --  107.75  61.00-120.00  146
 48  \w     97.00 137.00   0.50    1.74    --  107.75  61.00 -60.00   80
 49  \w     98.00 130.00   0.50    1.74    --  107.75  45.00 -90.00   64
 50  \w    102.00 128.00   0.50    1.74    --  107.75  39.00-146.66   52
 51  \w     99.00 178.00   0.50    1.74    --  107.75  30.00-180.00  158
 52  \w     86.00 116.00   0.50    1.74    --  107.75  77.00   0.00   60
 53  \w     86.00 111.00   0.50    1.74    --  107.75  77.00  30.00   50
 54  \w     95.00 130.00   0.50    1.74    --  107.75  61.00  60.00   70
 55  \w    104.00 136.00   0.50    1.74    --  107.75  30.00  30.00   64
 56  \w     98.00 139.00   0.50    1.74    --  107.75  45.00  90.00   82
 57  \w    102.00 160.00   0.50    1.74    --  107.75  15.00 150.00  116
 58  \w     78.00 104.00   0.50    1.74    --   98.00  75.00  18.76   52
 59  \w     93.00 159.00   0.50    1.74    --  107.75  61.00   0.00  132
 60  \w     89.00 114.00   0.50    1.74    --  107.75  76.00 135.48   50
 61  \w     86.00 124.00   0.50    1.74    --  107.75  77.00 150.00   76
 62  \w     80.00 114.00   0.50    1.74    --  102.00  79.00 133.06   68
 63  \w     87.00 118.00   0.50    1.74    --  107.75  77.00  70.64   62
 64  \w     86.00 137.00   0.50    1.74    --  107.75  77.00 120.00  102
 65  \w     84.00 119.00   0.50    1.74    --  107.75  81.00 101.54   70
 66  \w     86.00 162.00   0.50    1.74    --  107.75  77.00  60.00  152
 67  \w     93.00 141.00   0.50    1.74    --  107.75  61.00 -30.00   96
 68  \w     86.00 132.00   0.50    1.74    --  107.75  77.00 -90.00   92
 69  \w     94.00 141.00   0.50    1.74    --  107.75  61.00-150.00   94
 70  \w     89.00 127.00   0.50    1.74    --  107.75  77.00-180.00   76
 71  \w     86.00 173.00   0.50    1.74    --  107.75  77.00-150.00  174
 72  \w     93.00 121.00   0.50    1.74    --  107.75  61.00-180.00   56
 73  \w     86.00 125.00   0.50    1.74    --  107.75  77.00-120.00   78
 74  \w     90.00 146.00   0.50    1.74    --  107.75  70.00 -76.75  112
 75  \w     86.00 112.00   0.50    1.74    --  107.75  77.00 -60.00   52
 76  \w     68.00  94.00   0.50    1.74    --   90.00  83.00 -43.86   52
 77  \w     43.00  69.00   0.50    0.44    --   62.00  72.00  65.33   52
 78  \w     48.00  74.00   0.50    0.44    --   70.00  77.00 118.75   52
 79  \w     49.00  74.00   0.50    0.44    --   70.00  76.00  94.74   50
 80  \w     39.00 122.00   0.50    0.44    --   48.30  19.00  90.00  166
 81  \w     86.00 173.00   0.50    1.74    --  107.75  77.00  90.00  174
 82  \w     90.00 129.00   0.50    1.74    --  107.75 -90.00  -8.74   78
 83  \w     88.00 119.00   0.50    1.74    --  107.75-129.00 -35.00   62
 84  \w     91.00 122.00   0.50    1.74    --  107.75-133.00  -2.58   62
 85  \w     83.00 109.00   0.50    1.74    --  107.75 -94.00  60.00   52
 86  \w     79.00 116.00   0.50    1.74    --  107.75-125.00  90.00   74
 87  \w    103.00 128.00   0.50    1.74    --  107.75-140.00 151.00   50
 88  \w     75.00 101.00   0.50    1.74    --  107.75-140.00 151.00   52
 89  \w     74.00 116.00   0.50    1.74    --  107.75-125.00 120.00   84
 90  \w     81.00 107.00   0.50    1.74    --  107.75-125.00 150.00   52
 91  \w     40.00 104.00   0.50    0.44    --   48.30-140.00 151.00  128
 92  \w     36.00  98.00   0.50    1.74    --  107.75 -77.00 120.00  124
 93  \w     82.00 108.00   0.50    1.74    --  107.75-125.00  30.00   52
 94  \w     74.00 116.00   0.50    1.74    --  107.75-125.00   0.00   84
 95  \w     88.00 114.00   0.50    1.74    --  107.75-125.00 -90.00   52
 96  \w     84.00 109.00   0.50    1.74    --  107.75 -94.00-120.00   50
 97  \w     79.00 116.00   0.50    1.74    --  107.75-125.00-150.00   74
 98  \w     88.00 114.00   0.50    1.74    --  107.75-125.00-180.00   52
 99  \w     72.00 105.00   0.50    1.74    --  107.75 -77.00-180.00   66
100  \w     76.00 116.00   0.50    1.74    --  107.75-125.00-120.00   80
101  \w     34.00  96.00   0.50    0.44    --   48.30-129.00 -35.00  124
102  \w     38.00  94.00   0.50    1.74    --  107.75 -77.00   0.00  112
103  \w     37.00  64.00   0.50    1.74    --  107.75 -61.00  90.00   54
104  \w     39.00  70.00   0.50    1.74    --  107.75 -61.00  60.00   62
105  \w     46.00  72.00   0.50    1.74    --  107.75 -81.00  21.43   52
106  \w     42.00  71.00   0.50    1.74    --  107.75 -61.00 -60.00   58
107  \w     44.00  83.00   0.50    1.74    --  107.75 -94.00 -90.00   78
108  \w     39.00  64.00   0.50    1.74    --  107.75-125.00-150.00   50
109  \w     36.00  65.00   0.50    1.74    --  107.75-125.00-120.00   58
110  \w     45.00 113.00   0.50    1.74    --  107.75-118.00 -82.46  136
111  \w     44.00  70.00   0.50    1.74    --  107.75-125.00-180.00   52
112  \w     36.00  62.00   0.50    1.74    --  107.75 -77.00-180.00   52
113  \w     37.00  70.00   0.50    1.74    --  107.75 -77.00-150.00   66
114  \w     36.00 104.00   0.50    1.74    --  107.75 -77.00 -90.00  136
115  \w     42.00  68.00   0.50    1.74    --  107.75-133.00  -2.58   52
116  \w     38.00  79.00   0.50    1.74    --  107.75 -94.00  60.00   82
117  \w     37.00  63.00   0.50    1.74    --  107.75-125.00 120.00   52
118  \w     36.00  65.00   0.50    1.74    --  107.75-125.00 150.00   58
119  \w     36.00  61.00   0.50    1.74    --  107.75-125.00  90.00   50
120  \w     36.00  87.00   0.50    1.74    --  107.75 -90.00  -8.74  102
121  \w     36.00  66.00   0.50    1.74    --  107.75 -94.00-120.00   60
122  \w     40.00  67.00   0.50    1.74    --  107.75-125.00 -90.00   54
123  \w     39.00  89.00   0.50    1.74    --  107.75 -77.00 -60.00  100
124  \w     39.00  64.00   0.50    1.74    --  107.75-125.00   0.00   50
125  \w     36.00  61.00   0.50    1.74    --  107.75 -61.00 150.00   50
126  \w     20.00  46.00   0.50    0.44    --   46.00  89.00 163.02   52
127  \w     20.00  45.00   0.50    0.44    --   46.00  86.00 134.53   50
128  \w     20.00  45.00   0.50    0.44    --   46.00  86.00 105.03   50
129  \w     36.00  61.00   0.50    0.44    --   58.00  78.00  92.89   50
130  \w     48.00  74.00   0.50    0.44    --   70.00  77.00  29.60   52
131  \w     31.00  64.00   0.50    0.44    --   54.00  80.00  26.28   66
132  \w     27.00  87.00   0.50    0.44    --   50.00  80.00 -58.97  120
133  \w     49.00  87.00   0.50    0.44    --   70.00  76.00 -50.18   76
134  \w     48.00  74.00   0.50    0.44    --   70.00  77.00 -73.43   52
135  \w     49.00  74.00   0.50    0.44    --   70.00  76.00-106.96   50
136  \w     32.00  91.00   0.50    0.44    --   54.00  77.00 -18.92  118
137  \w     33.00  89.00   0.50    0.44    --   54.00  77.00 -95.21  112
138  \w     70.00 117.00   0.50    1.74    --   94.00  82.00-179.44   94
139  \w     36.00  62.00   0.50    0.44    --   58.00  77.00-146.89   52
140  \w     34.00  61.00   0.50    0.44    --   58.00  82.00-137.93   54
141  \w     15.00  40.00   0.50    0.44    --   42.00  88.00 -88.48   50
142  \w      1.00  26.00   0.50    0.44    --   30.00  95.00 -21.42   50
143  \w     -5.00  21.00   0.50    0.44    --   26.00 100.00-129.44   52
144  \w    -25.00   0.00   0.50    0.44    --   14.00 111.00-173.34   50
145  \w    -42.00 -12.00   0.50    0.44    --    6.00 128.00-128.76   60
146  \w    -76.00 -51.00   0.50    0.44    --  -48.30 140.00-149.00   50
147  \w    -84.00 -59.00   0.50    1.74    --  -86.25 140.00-149.00   50
148  \w    -94.00 -12.00   0.50    0.44    --  -48.30 129.00  37.00  164
149  \w    -78.00 -53.00   0.50    1.74    --  -86.25 129.00  37.00   50
150  \w   -114.00 -37.00   0.50    0.44    --  -48.30 -37.00-120.00  154
151  \w    -69.00 -43.00   0.50    0.44    --  -66.00 -82.00 -76.51   52
152  \w    -64.00 -38.00   0.50    0.44    --  -62.00 -82.00 -10.29   52
153  \w    -77.00 -45.00   0.50    1.74    --  -70.00 -83.00 -10.80   64
154  \w    -75.00 -50.00   0.50    1.74    --  -74.00 -81.00 -31.49   50
155  \w    -82.00 -57.00   0.50    1.74    --  -78.00 -75.00  37.41   50
156  \w    -75.00 -49.00   0.50    1.74    --  -74.00 -83.00  70.79   52
157  \w    -79.00 -39.00   0.50    0.44    --  -62.00 -79.00 115.56   80
158  \w    -55.00 -29.00   0.50    0.44    --  -54.00 -83.00 152.34   52
159  \w    -72.00 -46.00   0.50    1.74    --  -70.00 -83.00 159.49   52
160  \w    -77.00 -45.00   0.50    0.44    --  -66.00 -74.00 165.60   64
161  \w    -80.00 -54.00   0.50    1.74    --  -78.00 -82.00 167.84   52
162  \w    -88.00 -53.00   0.50    1.74    --  -78.00 -83.00 133.70   70
163  \w    -91.00 -65.00   0.50    1.74    --  -86.25 -77.00 120.00   52
164  \w    -92.00 -64.00   0.50    1.74    --  -86.25 -80.00 115.03   56
165  \w   -108.00 -82.00   0.50    0.44    --  -48.30-140.00 151.00   52
166  \w    -87.00 -61.00   0.50    1.74    --  -86.00 -83.00 -38.29   52
167  \w    -90.00 -64.00   0.50    1.74    --  -86.25 -78.00 -99.28   52
168  \w    -77.00 -51.00   0.50    1.74    --  -74.00 -82.00-136.19   52
169  \w    -76.00 -50.00   0.50    1.74    --  -74.00 -82.00-160.31   52
170  \w    -79.00 -54.00   0.50    1.74    --  -78.00 -82.00-162.35   50
171  \w    -89.00 -63.00   0.50    1.74    --  -86.25 -80.00-131.21   52
172  \w    -90.00 -64.00   0.50    1.74    --  -86.25 -77.00-120.00   52
173  \w    -93.00 -66.00   0.50    1.74    --  -86.25 -72.00-150.51   54
174  \w    -89.00 -64.00   0.50    1.74    --  -86.25 -77.00 -90.00   50
175  \w    -90.00 -64.00   0.50    1.74    --  -86.25 -78.00 -67.93   52
176  \w   -101.00 -61.00   0.50    1.74    --  -82.00 -75.00 -28.15   80
177  \w    -91.00 -65.00   0.50    1.74    --  -86.25 -75.00   1.25   52
178  \w    -95.00 -68.00   0.50    1.74    --  -86.25 -69.00   1.86   54
179  \w    -92.00 -66.00   0.50    1.74    --  -86.25 -74.00  39.84   52
180  \w   -109.00 -64.00   0.50    1.74    --  -86.25 -77.00  30.00   90
181  \w   -118.00 -93.00   0.50    0.44    --  -48.30-129.00 -35.00   50
182  \w   -137.00-112.00   0.50    1.74    --  -86.25-129.00 -35.00   50
183  \w   -126.00-100.00   0.50    0.44    --  -66.00 -82.00 -76.51   52
184  \w   -133.00 -99.00   0.50    1.74    --  -86.25 -69.00   1.86   68
185  \w   -157.00 -65.00   0.50    1.74    --  -86.25 -75.00 130.85  184
186  \w   -105.00 -65.00   0.50    1.74    --  -86.25 -75.00 155.83   80
187  \w   -133.00-108.00   0.50    1.74    --  -86.25-140.00 151.00   50
188  \w   -126.00 -61.00   0.50    1.74    --  -82.00 -74.00-179.89  130
189  \w     36.00  63.00   0.50    1.74    --  107.75 -61.00-180.00   54
;
_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      -0.0035310000
_diffrn_orient_matrix_UB_12      -0.0634123000
_diffrn_orient_matrix_UB_13      -0.0023344000
_diffrn_orient_matrix_UB_21      -0.0319398000
_diffrn_orient_matrix_UB_22      -0.0012187000
_diffrn_orient_matrix_UB_23      0.0659523000
_diffrn_orient_matrix_UB_31      -0.1044015000
_diffrn_orient_matrix_UB_32      0.0025281000
_diffrn_orient_matrix_UB_33      -0.0270527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            367185
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.077
_diffrn_reflns_theta_min         1.820
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.26a (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       plate
_exptl_crystal_F_000             3000
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 13431 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1931
_refine_ls_number_reflns         30389
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+1.6847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.922
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.919
_reflns_number_gt                29427
_reflns_number_total             30389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c03492_si_002.cif
_cod_data_source_block           rakh1_abs
_cod_database_code               4518134
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C192H164Al2B2N4O14
_chemical_oxdiff_usercomment     'Crystallized from THF.'
_reflns_odcompleteness_completeness 98.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.89
_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.a Secondary CH2 refined with riding coordinates:
 C112(H11A,H11B), C113(H11C,H11D), C145(H14A,H14B), C146(H14C,H14D), C161(H16D,
 H16E), C162(H16F,H16G), C163(H16H,H16I), C164(H16J,H16K), C165(H16L,H16M),
 C166(H16N,H16O), C167(H16P,H16Q), C168(H16R,H16S), C212(H21A,H21B), C213(H21C,
 H21D), C245(H24A,H24B), C246(H24C,H24D), C261(H26D,H26E), C262(H26F,H26G),
 C263(H26H,H26I), C264(H26J,H26K), C265(H26L,H26M), C266(H26N,H26O), C267(H26P,
 H26Q), C268(H26R,H26S), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB),
 C4S(H4SA,H4SB), C5S(H5SA,H5SB), C6S(H6SA,H6SB), C7S(H7SA,H7SB), C8S(H8SA,H8SB)
2.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C106(H106), C107(H107), C109(H109), C110(H110),
 C115(H115), C120(H120), C122(H122), C123(H123), C125(H125), C126(H126),
 C127(H127), C128(H128), C133(H133), C134(H134), C135(H135), C136(H136),
 C138(H138), C139(H139), C141(H141), C143(H143), C148(H148), C149(H149),
 C155(H155), C156(H156), C158(H158), C159(H159), C203(H203), C204(H204),
 C206(H206), C207(H207), C209(H209), C210(H210), C215(H215), C220(H220),
 C222(H222), C223(H223), C225(H225), C226(H226), C227(H227), C228(H228),
 C233(H233), C234(H234), C235(H235), C236(H236), C238(H238), C239(H239),
 C241(H241), C243(H243), C248(H248), C249(H249), C255(H255), C256(H256),
 C258(H258), C259(H259), C170(H170), C171(H171), C172(H172), C173(H173),
 C174(H174), C176(H176), C177(H177), C178(H178), C179(H179), C180(H180),
 C182(H182), C183(H183), C184(H184), C185(H185), C186(H186), C188(H188),
 C189(H189), C190(H190), C191(H191), C192(H192), C270(H270), C271(H271),
 C272(H272), C273(H273), C274(H274), C276(H276), C277(H277), C278(H278),
 C279(H279), C280(H280), C282(H282), C283(H283), C284(H284), C285(H285),
 C286(H286), C288(H288), C289(H289), C290(H290), C291(H291), C292(H292)
2.c Idealised Me refined as rotating group:
 C101(H10A,H10B,H10C), C160(H16A,H16B,H16C), C201(H20A,H20B,H20C), C260(H26A,
 H26B,H26C)
;
_shelx_res_checksum              92246
_shelx_hkl_checksum              91272
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.600
_oxdiff_exptl_absorpt_empirical_full_min 0.723