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_7133782
_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, 1[C7H8]'
_chemical_formula_sum            'C79 H100 Al2 N4'
_chemical_formula_weight         1159.58
_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
_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                75.831(3)
_cell_angle_beta                 82.021(3)
_cell_angle_gamma                75.106(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1124(4)
_cell_length_b                   13.4322(4)
_cell_length_c                   21.3152(7)
_cell_measurement_reflns_used    13436
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1180
_cell_measurement_theta_min      3.5160
_cell_volume                     3506.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9832
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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   -104.00 -53.00   1.00   15.50    --  -33.50 -19.00 -30.00   51
  2  \w    -99.00 -71.00   1.00   15.50    --  -33.50 -57.00 -90.00   28
  3  \w    -52.00 -11.00   1.00   15.50    --  -33.50 -19.00 -30.00   41
  4  \w    -50.00 -17.00   1.00   15.50    --  -33.50 -57.00 -90.00   33
  5  \w     36.00  72.00   1.00   15.50    --   36.21 -99.00  90.00   36
  6  \w      5.00  74.00   1.00   15.50    --   36.21 -99.00-120.00   69
  7  \w    -33.00  40.00   1.00   15.50    --   36.21 -37.00 150.00   73
  8  \w     26.00 105.00   1.00   15.50    --   36.21  37.00 -30.00   79
  9  \w    -29.00  55.00   1.00   15.50    --   36.21 -37.00   0.00   84
 10  \w     49.00  74.00   1.00   15.50    --   36.21 -99.00   0.00   25
 11  \w     63.00 108.00   1.00   15.50    --   36.21 178.00 -90.00   45
 12  \w     40.00  91.00   1.00   15.50    --   36.21  57.00 120.00   51
 13  \w     69.00 104.00   1.00   15.50    --   36.21-178.00  90.00   35
 14  \w     75.00 107.00   1.00   63.50    --  108.00-111.00 -30.00   32
 15  \w    103.00 130.00   1.00   63.50    --  108.00  77.00-180.00   27
 16  \w    100.00 126.00   1.00   63.50    --  108.00 -77.00  60.00   26
 17  \w    108.00 150.00   1.00   63.50    --  108.00 111.00 -90.00   42
 18  \w     90.00 158.00   1.00   63.50    --  108.00  61.00 -30.00   68
 19  \w     70.00 177.00   1.00   63.50    --  108.00  15.00  60.00  107
 20  \w    127.00 176.00   1.00   63.50    --  108.00  77.00 120.00   49
 21  \w     44.00 124.00   1.00   63.50    --  108.00 -45.00 -30.00   80
 22  \w    106.00 150.00   1.00   63.50    --  108.00 111.00  60.00   44
 23  \w     53.00 106.00   1.00   63.50    --  108.00 -94.00   0.00   53
 24  \w     57.00  87.00   1.00   63.50    --  108.00 -77.00  60.00   30
 25  \w     92.00 149.00   1.00   63.50    --  108.00  45.00 120.00   57
 26  \w    125.00 170.00   1.00   63.50    --  108.00 111.00  30.00   45
 27  \w     51.00 109.00   1.00   63.50    --  108.00-111.00 150.00   58
 28  \w     40.00 122.00   1.00   63.50    --  108.00 -45.00 120.00   82
 29  \w     82.00 122.00   1.00   63.50    --  108.00 -61.00-150.00   40
 30  \w     61.00 106.00   1.00   63.50    --  108.00-111.00-120.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0418921000
_diffrn_orient_matrix_UB_12      0.0426184000
_diffrn_orient_matrix_UB_13      0.0497282000
_diffrn_orient_matrix_UB_21      0.1072475000
_diffrn_orient_matrix_UB_22      -0.0794271000
_diffrn_orient_matrix_UB_23      -0.0054440000
_diffrn_orient_matrix_UB_31      0.0402598000
_diffrn_orient_matrix_UB_32      0.0816442000
_diffrn_orient_matrix_UB_33      -0.0555950000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24756
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.224
_diffrn_reflns_theta_min         3.489
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_description       block
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.269
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         13471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0601P)^2^+0.9761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11239
_reflns_number_total             13471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03904a3.cif
_cod_data_source_block           exp_585_auto
_cod_depositor_comments
'Adding full bibliography for 7133782--7133785.cif.'
_cod_database_code               7133782
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Al2 C70 H90 N4'
_chemical_oxdiff_usercomment     IS-064
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C36(H36), C30(H30), C33(H33), C47(H47), C70(H70), C10(H10), C67(H67), C7(H7),
 C50(H50), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C65(H65), C23(H23), C55(H55), C15(H15), C18(H18),
 C63(H63), C45(H45), C56(H56), C43(H43), C37(H37), C59(H59), C38(H38), C44(H44),
  C64(H64), C25(H25), C58(H58), C24(H24), C3(H3), C5(H5), C4(H4), C74(H74),
 C73(H73), C78(H78), C77(H77), C76(H76)
2.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C48(H48A,H48B,
 H48C), C40(H40A,H40B,H40C), C72(H72A,H72B,H72C), C51(H51A,H51B,H51C), C71(H71A,
 H71B,H71C), C20(H20A,H20B,H20C), C69(H69A,H69B,H69C), C39(H39A,H39B,H39C),
 C60(H60A,H60B,H60C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C68(H68A,H68B,H68C),
 C28(H28A,H28B,H28C), C11(H11A,H11B,H11C), C52(H52A,H52B,H52C), C29(H29A,H29B,
 H29C), C12(H12A,H12B,H12C), C79(H79A,H79B,H79C)
;
_shelx_res_checksum              80247
_shelx_hkl_checksum              68862
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.819