Probing the reactivity of a transient Al(I) species with substituted arenes.
Squire, Imogen; Tritto, Michelangelo; Morell, Juliana; Bakewell, Clare; Chemical communications (Cambridge, England) 60 (2024) 12908–12911; doi:10.1039/d4cc03904a

data_7133783
_publ_section_title
;
 Probing the reactivity of a transient Al(I) species with substituted
 arenes.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12908
_journal_page_last               12911
_journal_paper_doi               10.1039/d4cc03904a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C72 H92 Al2 N4, C6 H9.913'
_chemical_formula_sum            'C78 H101.91 Al2 N4'
_chemical_formula_weight         1149.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-06-25 deposited with the CCDC.	2024-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.4350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.1421(3)
_cell_length_b                   16.4913(2)
_cell_length_c                   19.8962(2)
_cell_measurement_reflns_used    27917
_cell_measurement_temperature    150.05(12)
_cell_measurement_theta_max      78.4040
_cell_measurement_theta_min      3.3660
_cell_volume                     7066.32(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.05(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_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    -11.00  25.00   0.50    5.00    --  -42.00  56.00  90.00   72
  2  \w    -52.00 -26.00   0.50    5.00    --  -42.00  56.00  90.00   52
  3  \w   -111.00 -71.00   0.50    5.00    --  -42.00 -56.00 -51.00   80
  4  \w    -63.00 -28.00   0.50    5.00    --  -42.00 -56.00 -51.00   70
  5  \w     34.00  68.00   0.50    5.00    --   48.48  56.00  90.00   68
  6  \w    141.00 167.00   0.50    5.00    --  100.18  56.00  90.00   52
  7  \w     93.00 118.00   0.50    5.00    --  100.18  56.00  90.00   50
  8  \w     43.00 125.00   0.50    5.00    --  111.08 -56.00 -51.00  164
  9  \w    -55.00 -29.00   0.50    5.00    --   14.00 155.00-156.63   52
 10  \w    -13.00  13.00   0.50    5.00    --   22.00 101.00 -65.24   52
 11  \w    -83.00 -37.00   0.50    5.00    --  -42.00 125.00 120.00   92
 12  \w    -77.00 -24.00   0.50    5.00    --  -42.00 125.00 -60.00  106
 13  \w   -116.00 -79.00   0.50    5.00    --  -42.00 -19.00   0.00   74
 14  \w    -68.00  -9.00   0.50    5.00    --  -42.00 -19.00   0.00  118
 15  \w     17.00  42.00   0.50    5.00    --   46.00  89.00-111.18   50
 16  \w     16.00  41.00   0.50    5.00    --   46.00  91.00 -11.83   50
 17  \w     15.00  41.00   0.50    5.00    --   46.00  92.00 162.64   52
 18  \w     16.00  41.00   0.50    5.00    --   46.00  91.00  68.40   50
 19  \w     44.00  71.00   0.50    5.00    --   48.48  38.00  90.00   54
 20  \w    -20.00  45.00   0.50    5.00    --   48.48 -56.00 -51.00  130
 21  \w     38.00  80.00   0.50    5.00    --   48.48-125.00-180.00   84
 22  \w     34.00  61.00   0.50    5.00    --   54.00  76.00  17.22   54
 23  \w     34.00  96.00   0.50    5.00    --   54.00  76.00  87.67  124
 24  \w     33.00  59.00   0.50    5.00    --   54.00  76.00 -68.71   52
 25  \w     36.00  72.00   0.50    5.00    --   58.00  77.00 -21.40   72
 26  \w     42.00  80.00   0.50    5.00    --   62.00  75.00  49.46   76
 27  \w     43.00  69.00   0.50    5.00    --   62.00  74.00  27.71   52
 28  \w     42.00  89.00   0.50    5.00    --   62.00  74.00 162.72   94
 29  \w     44.00  69.00   0.50    5.00    --   66.00  77.00 -98.84   50
 30  \w     78.00 130.00   0.50    5.00    --   66.00  76.00 128.07  104
 31  \w     46.00  73.00   0.50    5.00    --   66.00  76.00 128.07   54
 32  \w     44.00  72.00   0.50    5.00    --   66.00  77.00  92.71   56
 33  \w     45.00  71.00   0.50    5.00    --   66.00  75.00-174.64   52
 34  \w     45.00 127.00   0.50    5.00    --   66.00  76.00-139.74  164
 35  \w    104.00 130.00   0.50    5.00    --   66.00  75.00-174.64   52
 36  \w    105.00 130.00   0.50    5.00    --   66.00  74.00 164.96   50
 37  \w     46.00  74.00   0.50    5.00    --   66.00  74.00 164.96   56
 38  \w     98.00 132.00   0.50    5.00    --   70.00  77.00  57.09   68
 39  \w     48.00  90.00   0.50    5.00    --   70.00  77.00  57.09   84
 40  \w     93.00 119.00   0.50    5.00    --   70.00  77.00 -27.79   52
 41  \w     48.00  89.00   0.50    5.00    --   70.00  77.00 -27.79   82
 42  \w     49.00  75.00   0.50    5.00    --   70.00  75.00 -68.17   52
 43  \w     98.00 124.00   0.50    5.00    --   70.00  76.00  99.90   52
 44  \w     49.00  75.00   0.50    5.00    --   70.00  76.00  99.90   52
 45  \w     52.00 104.00   0.50    5.00    --   74.00  77.00 -18.68  104
 46  \w     65.00 150.00   0.50    5.00    --   82.00  68.00 -80.33  170
 47  \w     72.00 155.00   0.50    5.00    --   86.00  63.00  11.70  166
 48  \w    112.00 150.00   0.50    5.00    --   86.00  75.00  29.93   76
 49  \w     69.00  94.00   0.50    5.00    --   86.00  65.00 174.57   50
 50  \w     65.00  91.00   0.50    5.00    --   86.00  75.00  29.93   52
 51  \w     86.00 125.00   0.50    5.00    --  100.18  61.00-150.00   78
 52  \w     78.00 151.00   0.50    5.00    --  100.18  77.00 120.00  146
 53  \w     78.00 108.00   0.50    5.00    --  100.18  77.00 -90.00   60
 54  \w     78.00 103.00   0.50    5.00    --  100.18  77.00  60.00   50
 55  \w    137.00 163.00   0.50    5.00    --  100.18  77.00 -30.00   52
 56  \w     81.00 114.00   0.50    5.00    --  100.18  77.00 -30.00   66
 57  \w     79.00 159.00   0.50    5.00    --  100.18  77.00  30.00  160
 58  \w     78.00 104.00   0.50    5.00    --  100.18  77.00  90.00   52
 59  \w    121.00 160.00   0.50    5.00    --  100.18  77.00 -60.00   78
 60  \w     78.00 104.00   0.50    5.00    --  100.18  77.00 -60.00   52
 61  \w     87.00 122.00   0.50    5.00    --  100.18  61.00 120.00   70
 62  \w    119.00 161.00   0.50    5.00    --  100.18  77.00-120.00   84
 63  \w     78.00 106.00   0.50    5.00    --  100.18  77.00-120.00   56
 64  \w     37.00 122.00   0.50    5.00    --  100.18 -77.00 120.00  170
 65  \w    115.00 157.00   0.50    5.00    --  100.18  77.00-180.00   84
 66  \w    127.00 163.00   0.50    5.00    --  100.18  77.00  60.00   72
 67  \w     81.00 164.00   0.50    5.00    --  100.18  77.00 150.00  166
 68  \w     78.00 104.00   0.50    5.00    --  100.18  77.00-180.00   52
 69  \w     90.00 115.00   0.50    5.00    --  100.18  61.00 -30.00   50
 70  \w     85.00 111.00   0.50    5.00    --  100.18  61.00-120.00   52
 71  \w     42.00 105.00   0.50    5.00    --  100.18 -95.00 -90.00  126
 72  \w     29.00  72.00   0.50    5.00    --  100.18 -56.00 -51.00   86
 73  \w     55.00 105.00   0.50    5.00    --  100.18 -95.00  30.00  100
 74  \w     78.00 164.00   0.50    5.00    --  100.18  77.00-150.00  172
 75  \w    144.00 175.00   0.50    5.00    --  111.08  77.00 -90.00   62
 76  \w     94.00 141.00   0.50    5.00    --  111.08  77.00 -90.00   94
 77  \w     49.00 105.00   0.50    5.00    --  111.08 -95.00  90.00  112
 78  \w    100.00 136.00   0.50    5.00    --  111.08  56.00  90.00   72
 79  \w     53.00 127.00   0.50    5.00    --  111.08 -61.00-150.00  148
 80  \w     56.00  89.00   0.50    5.00    --  111.08 -95.00   0.00   66
 81  \w    141.00 173.00   0.50    5.00    --  111.08  45.00 -30.00   64
 82  \w     87.00 112.00   0.50    5.00    --  111.08-125.00 -90.00   50
 83  \w     44.00  69.00   0.50    5.00    --  111.08-125.00 -90.00   50
 84  \w     62.00 105.00   0.50    5.00    --  111.08 -95.00 150.00   86
 85  \w     80.00 105.00   0.50    5.00    --  111.08 -95.00-180.00   50
 86  \w     48.00  74.00   0.50    5.00    --  111.08 -95.00-180.00   52
 87  \w    135.00 168.00   0.50    5.00    --  111.08  77.00-120.00   66
 88  \w     96.00 131.00   0.50    5.00    --  111.08  77.00-120.00   70
 89  \w    140.00 170.00   0.50    5.00    --  111.08  56.00  90.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, HyPix-Arc 100'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0455648000
_diffrn_orient_matrix_UB_12      -0.0704199000
_diffrn_orient_matrix_UB_13      0.0006324000
_diffrn_orient_matrix_UB_21      -0.0167904000
_diffrn_orient_matrix_UB_22      -0.0007620000
_diffrn_orient_matrix_UB_23      -0.0795934000
_diffrn_orient_matrix_UB_31      0.0525209000
_diffrn_orient_matrix_UB_32      -0.0613449000
_diffrn_orient_matrix_UB_33      0.0002595000
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84705
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.045
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       needle
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7463
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0637P)^2^+4.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6126
_reflns_number_total             7463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03904a3.cif
_cod_data_source_block           exp_542_auto
_cod_depositor_comments
'Adding full bibliography for 7133782--7133785.cif.'
_cod_database_code               7133783
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C78 H106 Al2 N4'
_chemical_oxdiff_usercomment
'IS088 batch of p-xylene crystals, slow evap from hexane'
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.828
_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. Restrained distances
 C38-C40 \\sim C38-C39
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40) = Uanis(C39)
4. Others
 Sof(C39)=Sof(H39)=1-FVAR(1)
 Sof(H38a)=Sof(H38b)=Sof(C40)=Sof(H40)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C12(H12), C15(H15), C31(H31), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 C38(H38a,H38b)
5.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C8(H8), C9(H9), C23(H23), C20(H20), C22(H22), C10(H10), C2(H2),
 C29(H29), C27(H27), C28(H28), C40(H40), C39(H39)
5.d Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C13(H13a,H13b,H13c), C4(H4a,H4b,H4c), C32(H32a,H32b,
 H32c), C35(H35a,H35b,H35c), C24(H24a,H24b,H24c), C33(H33a,H33b,H33c), C16(H16a,
 H16b,H16c), C17(H17a,H17b,H17c), C36(H36a,H36b,H36c), C37(H37a,H37b,H37c)
;
_shelx_res_checksum              55524
_shelx_hkl_checksum              65242
_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 2.213
_oxdiff_exptl_absorpt_empirical_full_min 0.645