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_1566892
_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         'C69 H82 Al2 N4, 1.5(C6 H6)'
_chemical_formula_sum            'C78 H91 Al2 N4'
_chemical_formula_weight         1138.50
_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'
_atom_sites_solution_hydrogens   geom
_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                 96.7420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.45280(10)
_cell_length_b                   15.23290(10)
_cell_length_c                   28.0296(3)
_cell_measurement_reflns_used    27338
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.0970
_cell_measurement_theta_min      2.9240
_cell_volume                     6552.29(9)
_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      99.9(6)
_diffrn_detector                 'HPAD area detector (HyPix 6000)'
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.959
_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     95.00 175.00   0.50    0.52    --  107.11  45.00  90.00  160
   2  \w     95.00 141.00   0.50    0.52    --  107.11 125.00  60.00   92
   3  \w     92.00 171.00   0.50    0.52    --  107.11  68.00   6.00  158
   4  \w    130.00 172.00   0.50    0.52    --  107.11  15.00 -30.00   84
   5  \w     50.00  75.00   0.50    0.13    --   47.45  68.00   6.00   50
   6  \w    -66.00  22.00   0.50    0.13    --  -47.45  68.00   6.00  176
   7  \w    -47.00 -14.00   0.50    0.52    --  -86.25  45.00  90.00   66
   8  \w    -55.00 -24.00   0.50    0.52    --  -86.25  68.00   6.00   62
   9  \w    -49.00 -15.00   0.50    0.52    --  -86.25  45.00-150.00   68
  10  \w    -43.00 -18.00   0.50    0.52    --  -86.25  45.00-180.00   50
  11  \w   -159.00-134.00   0.50    0.52    --  -86.25 -68.00-126.00   50
  12  \w   -120.00 -70.00   0.50    0.13    --  -47.45-125.00-180.00  100
  13  \w   -111.00 -29.00   0.50    0.13    --  -47.45 -68.00-126.00  164
  14  \w   -119.00 -70.00   0.50    0.13    --  -47.45-125.00   0.00   98
  15  \w     35.00  60.00   0.50    0.52    --  107.11 -61.00  90.00   50
  16  \w     44.00  77.00   0.50    0.52    --  107.11 -77.00  90.00   66
  17  \w     45.00  70.00   0.50    0.52    --  107.11 -61.00   0.00   50
  18  \w     36.00  62.00   0.50    0.52    --  107.11 -61.00  30.00   52
  19  \w      7.00  62.00   0.50    0.13    --   47.45 -68.00-126.00  110
  20  \w     36.00  68.00   0.50    0.52    --  107.11 -61.00 -60.00   64
  21  \w     48.00 101.00   0.50    0.52    --  107.11 -77.00 -90.00  106
  22  \w     35.00  82.00   0.50    0.52    --  107.11 -68.00-126.00   94
  23  \w     44.00 102.00   0.50    0.52    --  107.11 -94.00-150.00  116
  24  \w     43.00  69.00   0.50    0.52    --  107.11 -94.00  30.00   52
  25  \w     80.00 108.00   0.50    0.52    --  107.11 -94.00  30.00   56
  26  \w     83.00 108.00   0.50    0.52    --  107.11 -94.00 150.00   50
  27  \w     35.00  60.00   0.50    0.52    --  107.11 -94.00 150.00   50

;
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            49192
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.278
_diffrn_reflns_theta_min         2.880
_diffrn_source                   'microfocus sealed tube (PhotonJet)'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72338
_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    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         13342
_refine_ls_number_restraints     384
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+3.3679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11659
_reflns_number_total             13342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01436j2.cif
_cod_data_source_block           MaHa094_DeDh_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566892
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.903
_shelx_res_checksum              56299
_shelx_hkl_checksum              15308