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_1566890
_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         'C68 H80 Al2 N4'
_chemical_formula_sum            'C68 H80 Al2 N4'
_chemical_formula_weight         1007.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-16
_audit_creation_method           'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 117.934(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   16.9198(2)
_cell_length_b                   22.2833(2)
_cell_length_c                   17.4576(3)
_cell_measurement_reflns_used    19608
_cell_measurement_temperature    99.9(7)
_cell_measurement_theta_max      77.2950
_cell_measurement_theta_min      3.5480
_cell_volume                     5815.14(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.73a (Rigaku OD, 2020)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9891
_diffrn_measured_fraction_theta_max 0.9874
_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    -82.00  17.00   0.50    5.00    --  -47.45 102.00  19.00  198
  2  \w      5.00  74.00   0.50    5.00    --   47.45-102.00 -84.00  138
  3  \w   -122.00 -95.00   0.50   15.00    --  -86.25-102.00 -84.00   54
  4  \w    -73.00 -48.00   0.50   15.00    --  -86.25 102.00  19.00   50
  5  \w     78.00 109.00   0.50   15.00    --  107.75-102.00 -84.00   62
  6  \w    132.00 168.00   0.50   15.00    --  107.75 102.00  19.00   72
  7  \w   -120.00 -71.00   0.50    5.00    --  -47.45-125.00-180.00   98
  8  \w    -12.00  28.00   0.50    5.00    --  -47.45  19.00 -90.00   80
  9  \w   -112.00 -71.00   0.50    5.00    --  -47.45-125.00  90.00   82
 10  \w   -119.00 -75.00   0.50    5.00    --  -47.45-125.00   0.00   88
 11  \w   -101.00 -71.00   0.50    5.00    --  -47.45-125.00 -30.00   60
 12  \w    -50.00 -25.00   0.50   15.00    --  -86.25  45.00-120.00   50
 13  \w     35.00  60.00   0.50   15.00    --  107.75 -61.00 150.00   50
 14  \w     40.00  71.00   0.50   15.00    --  107.75 -61.00-180.00   62
 15  \w     36.00  70.00   0.50   15.00    --  107.75 -61.00 -90.00   68
 16  \w     59.00 105.00   0.50   15.00    --  107.75 -77.00-150.00   92
 17  \w     58.00  84.00   0.50   15.00    --  107.75-125.00 -90.00   52
 18  \w     45.00  90.00   0.50   15.00    --  107.75 -77.00  90.00   90
 19  \w     35.00  93.00   0.50   15.00    --  107.75 -77.00 150.00  116
 20  \w     35.00  60.00   0.50   15.00    --  107.75-125.00 120.00   50
 21  \w     35.00  70.00   0.50   15.00    --  107.75 -77.00   0.00   70
 22  \w    134.00 171.00   0.50   15.00    --  107.75 125.00 150.00   74
 23  \w     71.00  98.00   0.50   15.00    --  107.75 -94.00  90.00   54
 24  \w     91.00 176.00   0.50   15.00    --  107.75  61.00-120.00  170
 25  \w     96.00 127.00   0.50   15.00    --  107.75  45.00  90.00   62
 26  \w     56.00  99.00   0.50   15.00    --  107.75-125.00  30.00   86
 27  \w     84.00 109.00   0.50   15.00    --  107.75 -94.00 -30.00   50
 28  \w     47.00 102.00   0.50   15.00    --  107.75 -94.00 -60.00  110
 29  \w     36.00  71.00   0.50   15.00    --  107.75-125.00  90.00   70
 30  \w     76.00 107.00   0.50   15.00    --  107.75-125.00  90.00   62
 31  \w     98.00 125.00   0.50   15.00    --  107.75  30.00-150.00   54
 32  \w    138.00 178.00   0.50   15.00    --  107.75  30.00-150.00   80
 33  \w    118.00 144.00   0.50   15.00    --  107.75 125.00 -30.00   52
 34  \w     98.00 124.00   0.50   15.00    --  107.75 125.00 120.00   52
 35  \w    151.00 177.00   0.50   15.00    --  107.75 125.00 120.00   52
 36  \w     35.00  66.00   0.50   15.00    --  107.75 -61.00   0.00   62
 37  \w    103.00 129.00   0.50   15.00    --  107.75  30.00   0.00   52
 38  \w    123.00 176.00   0.50   15.00    --  107.75  45.00 120.00  106
 39  \w    102.00 127.00   0.50   15.00    --  107.75 125.00  90.00   50
 40  \w    142.00 168.00   0.50   15.00    --  107.75 125.00  90.00   52
 41  \w     75.00 100.00   0.50   15.00    --  107.75 -77.00 -90.00   50
 42  \w     35.00  61.00   0.50   15.00    --  107.75 -77.00 -60.00   52
 43  \w     37.00  69.00   0.50   15.00    --  107.75 -94.00 -30.00   64
 44  \w     45.00  71.00   0.50   15.00    --  107.75 -94.00 120.00   52
 45  \w     35.00  68.00   0.50   15.00    --  107.75 -61.00  90.00   66
 46  \w    142.00 176.00   0.50   15.00    --  107.75  45.00  90.00   68
 47  \w     38.00  64.00   0.50   15.00    --  107.75 -61.00 120.00   52
;
_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      -0.0523116000
_diffrn_orient_matrix_UB_12      0.0555774000
_diffrn_orient_matrix_UB_13      -0.0511175000
_diffrn_orient_matrix_UB_21      -0.0345117000
_diffrn_orient_matrix_UB_22      -0.0356728000
_diffrn_orient_matrix_UB_23      -0.0852651000
_diffrn_orient_matrix_UB_31      -0.0818157000
_diffrn_orient_matrix_UB_32      -0.0204651000
_diffrn_orient_matrix_UB_33      0.0096898000
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33342
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        77.1716
_diffrn_reflns_theta_max         77.5759
_diffrn_reflns_theta_min         3.0021
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73115
_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            colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0497P)^2^+5.4665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5462
_reflns_number_total             6108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01436j2.cif
_cod_data_source_block           MaHa090_DeDh_a
_cod_original_cell_volume        5815.16(14)
_cod_database_code               1566890
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.913
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              62329
_shelx_hkl_checksum              85391
_cell_oxdiff_length_a            16.9211(3)
_cell_oxdiff_length_b            22.2821(4)
_cell_oxdiff_length_c            17.4589(3)
_cell_oxdiff_angle_alpha         90.0300(13)
_cell_oxdiff_angle_beta          117.9438(19)
_cell_oxdiff_angle_gamma         89.9729(15)
_cell_oxdiff_volume              5815.16(18)
_cell_oxdiff_measurement_reflns_used 19662
_oxdiff_exptl_absorpt_empirical_full_min 0.737
_oxdiff_exptl_absorpt_empirical_full_max 1.385
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
0142329f865aea91393bc3a0a4a6ad7142034368395
;
_diffrn_oxdiff_digest_hkl
;
011e98fc0746db6f80e08bcc5b425495c1e63a
;
_reflns_odcompleteness_completeness 98.91
_reflns_odcompleteness_theta     77.17
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C68 H80 Al2 N4'
_chemical_oxdiff_usercomment     DD179