Generation of a transient base-stabilised arylalumylene for the facile deconstruction of aromatic molecules
Dhara, Debabrata; Jayaraman, Arumugam; Härterich, Marcel; Dewhurst, Rian; Braunschweig, Holger; Chemical Science  (2022) –; doi:10.1039/D2SC01436J

data_1566894
_publ_section_title
;
 Generation of a transient base-stabilised arylalumylene for the facile
 deconstruction of aromatic molecules
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01436J
_journal_year                    2022
_chemical_formula_moiety         'C62 H74 Al2 N4, C6 H14'
_chemical_formula_sum            'C68 H88 Al2 N4'
_chemical_formula_weight         1015.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2u (K.Radacki, 2005-21)'
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                112.4900(10)
_cell_angle_beta                 90.8700(10)
_cell_angle_gamma                105.4900(10)
_cell_formula_units_Z            2
_cell_length_a                   11.88400(10)
_cell_length_b                   15.41410(10)
_cell_length_c                   18.41380(10)
_cell_measurement_reflns_used    83611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8970
_cell_measurement_theta_min      2.6050
_cell_volume                     2977.13(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_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     16.00  41.00   0.50    0.21    --    6.00  65.00-138.09   50
   2  \w     12.00  37.00   0.50    0.21    --    2.00  65.00 -45.24   50
   3  \w     17.00  42.00   0.50    0.21    --    6.00  63.00 -51.58   50
   4  \w     17.00  42.00   0.50    0.21    --    6.00  63.00  19.75   50
   5  \w     21.00  46.00   0.50    0.21    --   10.00  62.00 -97.88   50
   6  \w     16.00  41.00   0.50    0.21    --    6.00  65.00  86.61   50
   7  \w     25.00  50.00   0.50    0.21    --   14.00  61.00 106.73   50
   8  \w     12.00  37.00   0.50    0.21    --    2.00  65.00 132.38   50
   9  \w     16.00  41.00   0.50    0.21    --    6.00  65.00 177.12   50
  10  \w     25.00  50.00   0.50    0.21    --   14.00  61.00  54.86   50
  11  \w     30.00  55.00   0.50    0.21    --   18.00  60.00  11.46   50
  12  \w     30.00  55.00   0.50    0.21    --   18.00  60.00 -15.51   50
  13  \w     30.00  55.00   0.50    0.21    --   18.00  60.00 -68.10   50
  14  \w     30.00  55.00   0.50    0.21    --   18.00  60.00-153.59   50
  15  \w     34.00  59.00   0.50    0.21    --   22.00  59.00-135.25   50
  16  \w     34.00  59.00   0.50    0.21    --   22.00  59.00-174.04   50
  17  \w     30.00  55.00   0.50    0.21    --   18.00  60.00-107.62   50
  18  \w     34.00  59.00   0.50    0.21    --   22.00  59.00 -93.68   50
  19  \w     34.00  59.00   0.50    0.21    --   22.00  59.00 -41.43   50
  20  \w     34.00  59.00   0.50    0.21    --   22.00  59.00  52.25   50
  21  \w     34.00  59.00   0.50    0.21    --   22.00  58.00   2.64   50
  22  \w     30.00  55.00   0.50    0.21    --   18.00  59.00  74.24   50
  23  \w     34.00  59.00   0.50    0.21    --   22.00  58.00 160.26   50
  24  \w     30.00  55.00   0.50    0.21    --   18.00  58.00 173.17   50
  25  \w     34.00  59.00   0.50    0.21    --   22.00  59.00 128.14   50
  26  \w     47.00  72.00   0.50    0.21    --   34.00  52.00  28.93   50
  27  \w     34.00  59.00   0.50    0.21    --   22.00  57.00 -21.43   50
  28  \w     51.00  76.00   0.50    0.21    --   38.00  52.00 -24.86   50
  29  \w     55.00  80.00   0.50    0.21    --   42.00  52.00 -54.71   50
  30  \w     47.00  72.00   0.50    0.21    --   34.00  52.00 -88.21   50
  31  \w     63.00  88.00   0.50    0.21    --   50.00  52.00-116.51   50
  32  \w     51.00  76.00   0.50    0.21    --   38.00  52.00 -76.80   50
  33  \w     59.00  84.00   0.50    0.21    --   46.00  52.00 -75.74   50
  34  \w     59.00  84.00   0.50    0.21    --   46.00  52.00 -50.53   50
  35  \w     52.00  77.00   0.50    0.21    --   38.00  51.00  12.32   50
  36  \w     59.00  84.00   0.50    0.21    --   46.00  52.00  51.94   50
  37  \w     52.00  77.00   0.50    0.21    --   38.00  51.00 135.27   50
  38  \w     38.00  80.00   0.50    0.21    --   85.25-134.00 126.99   84
  39  \w     74.00 100.00   0.50    0.21    --   82.33-115.00 -57.00   52
  40  \w     36.00  62.00   0.50    0.21    --   82.33-115.00 -57.00   52
  41  \w     35.00  60.00   0.50    0.21    --   71.56-115.00 -57.00   50
  42  \w     22.00  48.00   0.50    0.21    --   58.98-126.00-150.00   52
  43  \w     46.00 100.00   0.50    0.21    --   82.33-112.00-120.00  108
  44  \w     15.00  46.00   0.50    0.21    --   58.98-115.00 -57.00   62
  45  \w     34.00  99.00   0.50    0.21    --   82.33-112.00 -30.00  130
  46  \w     39.00 100.00   0.50    0.21    --   82.33-112.00   0.00  122
  47  \w     34.00  99.00   0.50    0.21    --   82.33-112.00  30.00  130
  48  \w     34.00  99.00   0.50    0.21    --   82.33-112.00 120.00  130
  49  \w     37.00 100.00   0.50    0.21    --   82.33-112.00 150.00  126
  50  \w     37.00 100.00   0.50    0.21    --   82.33-112.00  90.00  126
  51  \w     16.00  55.00   0.50    0.21    --   58.98 -95.00 150.00   78
  52  \w     40.00  85.00   0.50    0.21    --   82.33 -95.00 150.00   90
  53  \w     37.00 100.00   0.50    0.21    --   82.33-112.00  60.00  126
  54  \w     16.00  41.00   0.50    0.21    --   58.98 -95.00  30.00   50
  55  \w     16.00  44.00   0.50    0.21    --   58.98 -95.00-150.00   56
  56  \w     53.00 100.00   0.50    0.21    --   82.33-112.00-150.00   94
  57  \w    101.00 131.00   0.50    0.21    --   82.33  15.00-150.00   60
  58  \w     99.00 132.00   0.50    0.21    --   85.25  54.00-153.25   66
  59  \w     78.00 133.00   0.50    0.21    --   82.33  15.00  30.00  110
  60  \w    109.00 135.00   0.50    0.21    --   85.25  33.00 101.44   52
  61  \w     98.00 126.00   0.50    0.21    --   85.25  59.00  51.06   56
  62  \w    106.00 132.00   0.50    0.21    --   85.25 109.00  27.71   52
  63  \w    105.00 131.00   0.50    0.21    --   85.25 112.00 104.68   52
  64  \w    107.00 133.00   0.50    0.21    --   85.25 110.00-177.60   52
  65  \w    -36.00 -11.00   0.50    0.21    --  -10.00 121.00 105.98   50
  66  \w    -34.00  -9.00   0.50    0.21    --  -18.00 107.00 -12.00   50
  67  \w     -5.00  20.00   0.50    0.21    --  -10.00  77.00 -26.29   50
  68  \w    -83.00 -33.00   0.50    0.21    --  -79.50 133.00 168.18  100
  69  \w   -101.00 -32.00   0.50    0.21    --  -79.50 130.00 102.15  138
  70  \w    -61.00 -32.00   0.50    0.21    --  -79.50 124.00 121.41   58
  71  \w   -101.00 -32.00   0.50    0.21    --  -79.50 129.00 -23.88  138
  72  \w    -72.00 -21.00   0.50    0.21    --  -69.81 115.00  31.00  102
  73  \w    -94.00 -53.00   0.50    0.21    --  -76.36 115.00  31.00   82
  74  \w    -42.00 -16.00   0.50    0.21    --  -60.22 115.00  31.00   52
  75  \w    -67.00 -36.00   0.50    0.21    --  -79.50 128.00 -55.03   62
  76  \w    -68.00 -32.00   0.50    0.21    --  -79.50 122.00 -88.77   72
  77  \w    -69.00 -32.00   0.50    0.21    --  -79.50 126.00-171.64   74
  78  \w   -100.00 -37.00   0.50    0.21    --  -79.50 112.00-148.78  126
  79  \w    -87.00 -36.00   0.50    0.21    --  -79.50 100.00-114.21  102
  80  \w    -94.00 -38.00   0.50    0.21    --  -79.50 106.00 -55.76  112
  81  \w    -61.00 -32.00   0.50    0.21    --  -79.50 109.00 152.10   58
  82  \w    -97.00 -72.00   0.50    0.21    --  -79.50 109.00 152.10   50
  83  \w    -89.00 -64.00   0.50    0.21    --  -50.00 -47.00 127.57   50
  84  \w    -78.00 -52.00   0.50    0.21    --  -38.00 -52.00 158.03   52
  85  \w    -76.00 -50.00   0.50    0.21    --  -30.00 -52.00 131.77   52
  86  \w    -81.00 -55.00   0.50    0.21    --  -42.00 -52.00  36.51   52
  87  \w    -65.00 -39.00   0.50    0.21    --  -26.00 -52.00   7.35   52
  88  \w    -76.00 -51.00   0.50    0.21    --  -38.00 -51.00   4.37   50
  89  \w    -79.00 -53.00   0.50    0.21    --  -38.00 -52.00  -7.27   52
  90  \w    -93.00 -67.00   0.50    0.21    --  -50.00 -52.00-171.17   52
  91  \w    -80.00 -55.00   0.50    0.21    --  -42.00 -51.00-164.91   50
  92  \w    -72.00 -46.00   0.50    0.21    --  -30.00 -49.00-136.14   52
  93  \w    -78.00 -52.00   0.50    0.21    --  -38.00 -50.00 -88.81   52
  94  \w    -75.00 -49.00   0.50    0.21    --  -34.00 -51.00 -29.78   52
  95  \w    -71.00 -45.00   0.50    0.21    --  -30.00 -49.00  35.46   52
  96  \w    -69.00 -44.00   0.50    0.21    --  -30.00 -49.00  72.51   50
  97  \w    -71.00 -45.00   0.50    0.21    --  -30.00 -48.00  92.24   52
  98  \w    -82.00 -56.00   0.50    0.21    --  -42.00 -49.00 148.96   52
  99  \w   -120.00 -94.00   0.50    0.21    --  -79.50 -64.00 -23.53   52
 100  \w   -122.00 -94.00   0.50    0.21    --  -79.50 -64.00 -35.43   56
 101  \w   -122.00 -92.00   0.50    0.21    --  -79.50 -63.00 -96.04   60
 102  \w   -118.00 -92.00   0.50    0.21    --  -79.50 -63.00-176.97   52
 103  \w   -118.00 -92.00   0.50    0.21    --  -79.50 -63.00-162.82   52
 104  \w   -122.00 -90.00   0.50    0.21    --  -79.50 -62.00 -82.89   64
 105  \w   -117.00 -92.00   0.50    0.21    --  -79.50 -63.00  20.57   50
 106  \w   -123.00 -92.00   0.50    0.21    --  -79.50 -63.00  12.93   62
 107  \w   -124.00 -90.00   0.50    0.21    --  -79.50 -62.00  65.08   68
 108  \w   -117.00 -91.00   0.50    0.21    --  -79.50 -62.00 159.88   52
 109  \w   -115.00 -90.00   0.50    0.21    --  -79.50 -62.00 166.29   50
 110  \w   -120.00 -91.00   0.50    0.21    --  -79.50 -62.00 146.75   58
 111  \w   -120.00 -94.00   0.50    0.21    --  -79.50 -64.00 136.45   52
 112  \w   -124.00 -89.00   0.50    0.21    --  -78.00 -61.00  -4.54   70
 113  \w   -116.00 -91.00   0.50    0.21    --  -79.50 -60.00 -23.44   50
 114  \w   -114.00 -89.00   0.50    0.21    --  -78.00 -60.00  22.97   50
 115  \w   -125.00 -91.00   0.50    0.21    --  -79.50 -60.00 -11.18   68
 116  \w   -114.00 -89.00   0.50    0.21    --  -78.00 -61.00-135.84   50
 117  \w   -115.00 -89.00   0.50    0.21    --  -78.00 -61.00-148.24   52
 118  \w   -113.00 -87.00   0.50    0.21    --  -74.00 -60.00-169.63   52
 119  \w   -124.00 -91.00   0.50    0.21    --  -79.50 -61.00-138.54   66
 120  \w   -118.00 -92.00   0.50    0.21    --  -79.50 -60.00 -18.76   52
 121  \w   -115.00 -89.00   0.50    0.21    --  -78.00 -60.00 114.45   52
 122  \w   -119.00 -93.00   0.50    0.21    --  -79.50 -60.00 111.78   52
 123  \w   -113.00 -87.00   0.50    0.21    --  -74.00 -60.00 135.88   52
 124  \w   -116.00 -91.00   0.50    0.21    --  -79.50 -60.00 133.98   50
 125  \w   -117.00 -91.00   0.50    0.21    --  -79.50 -60.00  90.76   52
 126  \w   -121.00 -89.00   0.50    0.21    --  -78.00 -60.00  72.18   64
 127  \w   -125.00 -91.00   0.50    0.21    --  -79.50 -60.00 -65.28   68
 128  \w   -122.00 -91.00   0.50    0.21    --  -79.50 -60.00-115.07   62
 129  \w   -118.00 -92.00   0.50    0.21    --  -79.50 -60.00-176.55   52
 130  \w   -117.00 -91.00   0.50    0.21    --  -79.50 -59.00-157.48   52
 131  \w   -111.00 -86.00   0.50    0.21    --  -74.00 -59.00-131.83   50
 132  \w   -116.00 -90.00   0.50    0.21    --  -78.00 -59.00 -95.79   52
 133  \w   -117.00 -91.00   0.50    0.21    --  -79.50 -59.00 -56.12   52
 134  \w   -112.00 -86.00   0.50    0.21    --  -74.00 -58.00 -35.68   52
 135  \w   -125.00 -90.00   0.50    0.21    --  -78.00 -58.00  30.72   70
 136  \w   -118.00 -92.00   0.50    0.21    --  -79.50 -57.00  41.45   52
 137  \w   -126.00 -92.00   0.50    0.21    --  -79.50 -57.00  45.68   68
 138  \w   -121.00 -93.00   0.50    0.21    --  -79.50 -58.00  82.79   56
 139  \w   -116.00 -91.00   0.50    0.21    --  -79.50 -59.00  98.59   50
 140  \w   -116.00 -90.00   0.50    0.21    --  -78.00 -58.00 146.88   52
 141  \w   -110.00 -84.00   0.50    0.21    --  -70.00 -57.00  97.19   52
 142  \w   -120.00 -92.00   0.50    0.21    --  -79.50 -57.00 172.14   56
 143  \w   -112.00 -86.00   0.50    0.21    --  -74.00 -57.00  47.60   52
 144  \w   -114.00 -88.00   0.50    0.21    --  -74.00 -55.00  91.22   52
 145  \w   -116.00 -87.00   0.50    0.21    --  -74.00 -57.00 -46.95   58
 146  \w   -123.00 -96.00   0.50    0.21    --  -79.50 -57.00 -51.91   54
 147  \w   -126.00 -92.00   0.50    0.21    --  -79.50 -53.00-131.97   68
 148  \w   -121.00 -87.00   0.50    0.21    --  -74.00 -56.00 -76.79   68
 149  \w   -113.00 -84.00   0.50    0.21    --  -70.00 -55.00 -65.17   58
 150  \w    -97.00 -71.00   0.50    0.21    --  -58.00 -52.00 -71.11   52
 151  \w    -92.00 -67.00   0.50    0.21    --  -54.00 -52.00  65.18   50
 152  \w    -95.00 -69.00   0.50    0.21    --  -54.00 -52.00  97.87   52
 153  \w   -110.00 -84.00   0.50    0.21    --  -70.00 -55.00 118.64   52
 154  \w    -94.00 -68.00   0.50    0.21    --  -54.00 -52.00 174.14   52
 155  \w    -96.00 -71.00   0.50    0.21    --  -58.00 -52.00  42.76   50
 156  \w    -92.00 -67.00   0.50    0.21    --  -54.00 -52.00 127.00   50
 157  \w    -93.00 -67.00   0.50    0.21    --  -54.00 -52.00 113.99   52
 158  \w    -98.00 -72.00   0.50    0.21    --  -58.00 -51.00  84.87   52
 159  \w    -96.00 -71.00   0.50    0.21    --  -58.00 -52.00 -12.43   50
 160  \w    -97.00 -71.00   0.50    0.21    --  -58.00 -51.00 -24.68   52
 161  \w    -96.00 -71.00   0.50    0.21    --  -58.00 -52.00-143.29   50
 162  \w    -96.00 -71.00   0.50    0.21    --  -58.00 -51.00-110.20   50
 163  \w   -101.00 -75.00   0.50    0.21    --  -62.00 -52.00 -42.62   52
 164  \w    -97.00 -72.00   0.50    0.21    --  -58.00 -50.00 -37.33   50
 165  \w   -102.00 -76.00   0.50    0.21    --  -62.00 -51.00  20.86   52
 166  \w   -101.00 -71.00   0.50    0.21    --  -58.00 -51.00 152.87   60
 167  \w   -100.00 -74.00   0.50    0.21    --  -58.00 -50.00 165.51   52
 168  \w    -98.00 -72.00   0.50    0.21    --  -58.00 -50.00  -3.96   52
 169  \w    -97.00 -72.00   0.50    0.21    --  -58.00 -50.00 -90.15   50
 170  \w    -94.00 -68.00   0.50    0.21    --  -54.00 -48.00 -68.41   52
 171  \w    -98.00 -72.00   0.50    0.21    --  -58.00 -49.00-129.44   52
 172  \w   -128.00-102.00   0.50    0.21    --  -79.50-117.00-117.75   52
 173  \w   -124.00 -91.00   0.50    0.21    --  -79.50-140.00 -45.52   66
 174  \w   -126.00 -97.00   0.50    0.21    --  -79.50-130.00 -27.25   58
 175  \w   -128.00-103.00   0.50    0.21    --  -79.50-119.00 -20.59   50
 176  \w   -126.00 -93.00   0.50    0.21    --  -79.50-133.00  10.27   66
 177  \w   -128.00 -99.00   0.50    0.21    --  -79.50-120.00 150.71   58
 178  \w   -121.00 -90.00   0.50    0.21    --  -79.50-138.00  92.03   62
 179  \w   -128.00 -98.00   0.50    0.21    --  -79.50-118.00 170.65   60
 180  \w   -126.00 -98.00   0.50    0.21    --  -79.50-136.00  79.84   56
 181  \w   -128.00-103.00   0.50    0.21    --  -79.50-118.00 -11.27   50
 182  \w   -123.00 -96.00   0.50    0.21    --  -79.50-118.00-161.91   54

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            129644
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.804
_diffrn_reflns_theta_min         2.620
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.73a (Rigaku Oxford Diffraction, 2020) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     688
_refine_ls_number_reflns         11861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+1.2026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10366
_reflns_number_total             11861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01436j2.cif
_cod_data_source_block           MaHa139_DeDh_a
_cod_original_cell_volume        2977.13(4)
_cod_database_code               1566894
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.882
_shelx_estimated_absorpt_t_max   0.942
_shelx_res_checksum              12597
_shelx_hkl_checksum              37857