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_1566889
_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         'C31 H39 Al N2'
_chemical_formula_sum            'C31 H39 Al N2'
_chemical_formula_weight         466.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2n (K.Radacki 2005-21)'
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.0260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.67310(10)
_cell_length_b                   13.6845(2)
_cell_length_c                   22.6164(3)
_cell_measurement_reflns_used    13227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.9700
_cell_measurement_theta_min      3.9180
_cell_volume                     2673.95(6)
_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-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      100.0(6)
_diffrn_detector                 'HPAD area detector (HyPix 6000)'
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_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     48.00  74.00   0.50    0.13    --   47.45  34.00 -97.00   52
   2  \w    106.00 178.00   0.50    0.51    --  107.75 125.00  90.00  144
   3  \w    103.00 178.00   0.50    0.51    --  107.75  34.00 -97.00  150
   4  \w     95.00 160.00   0.50    0.51    --  107.75  30.00-150.00  130
   5  \w    -26.00  26.00   0.50    0.13    --   47.45 -19.00 -60.00  104
   6  \w     41.00  70.00   0.50    0.51    --  107.75 -77.00   0.00   58
   7  \w     79.00 106.00   0.50    0.51    --  107.75 -77.00   0.00   54
   8  \w     46.00  71.00   0.50    0.51    --  107.75 -61.00   0.00   50
   9  \w     39.00  70.00   0.50    0.51    --  107.75 -61.00  60.00   62
  10  \w     56.00  82.00   0.50    0.51    --  107.75 -77.00  90.00   52
  11  \w     36.00  98.00   0.50    0.51    --  107.75 -77.00 150.00  124
  12  \w     36.00  89.00   0.50    0.51    --  107.75 -77.00 120.00  106
  13  \w     37.00  71.00   0.50    0.51    --  107.75 -61.00  30.00   68
  14  \w      6.00  33.00   0.50    0.13    --   47.45 -34.00 104.00   54
  15  \w     35.00  62.00   0.50    0.51    --  107.75 -61.00 -30.00   54
  16  \w     37.00  63.00   0.50    0.51    --  107.75 -61.00-120.00   52
  17  \w     45.00  71.00   0.50    0.51    --  107.75 -61.00-150.00   52
  18  \w    -24.00  27.00   0.50    0.13    --  -47.45  19.00-180.00  102
  19  \w    -16.00  27.00   0.50    0.13    --  -47.45  34.00 -97.00   86
  20  \w    -67.00 -25.00   0.50    0.51    --  -86.25  61.00 -30.00   84
  21  \w    -39.00 -14.00   0.50    0.51    --  -86.25  34.00 -97.00   50
  22  \w    -44.00 -14.00   0.50    0.51    --  -86.25  45.00  60.00   60
  23  \w     45.00 105.00   0.50    0.51    --  107.75 -94.00-180.00  120
  24  \w     40.00  66.00   0.50    0.51    --  107.75-125.00-180.00   52
  25  \w   -122.00 -87.00   0.50    0.13    --  -47.45 -34.00 104.00   70
  26  \w   -141.00-116.00   0.50    0.51    --  -86.25 -34.00 104.00   50
  27  \w    -67.00 -38.00   0.50    0.13    --  -47.45 -34.00 104.00   58
  28  \w   -120.00 -93.00   0.50    0.13    --  -47.45-125.00 -30.00   54
  29  \w   -114.00 -81.00   0.50    0.13    --  -47.45-125.00-150.00   66

;
_diffrn_measurement_device_type  'Rigaku OD XtaLAB Synergy-S'
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            19589
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.488
_diffrn_reflns_theta_min         3.779
_diffrn_source                   'microfocus sealed tube (PhotonJet)'
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66191
_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    1.159
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5475
_refine_ls_number_restraints     437
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0522P)^2^+0.7906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1011
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4900
_reflns_number_total             5475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01436j2.cif
_cod_data_source_block           MaHa101_DeDh_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1566889
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.837
_shelx_estimated_absorpt_t_max   0.969
_shelx_res_checksum              97680
_shelx_hkl_checksum              74281