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_7133784
_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[C6H14]'
_chemical_formula_sum            'C78 H106 Al2 N4'
_chemical_formula_weight         1153.701
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_Int_Tables_number      15
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-04 deposited with the CCDC.	2024-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.723(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5835(2)
_cell_length_b                   16.8300(2)
_cell_length_c                   51.4307(5)
_cell_measurement_reflns_used    16610
_cell_measurement_temperature    150(3)
_cell_measurement_theta_max      76.6310
_cell_measurement_theta_min      3.6970
_cell_volume                     14255.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.60a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.60a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 100'
_diffrn_measured_fraction_theta_full 0.9963
_diffrn_measured_fraction_theta_max 0.9486
_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     44.00  73.00   0.50    4.66    --   99.84 -86.00-157.00   58
  2  \w     75.00 126.00   0.50    4.66    --   99.84 -86.00-157.00  102
  3  \w    106.00 131.00   0.50    4.66    --   99.84  86.00 -38.00   50
  4  \w     34.00  60.00   0.50    4.66    --   49.53-125.00  90.00   52
  5  \w     34.00  59.00   0.50    4.66    --   49.53 -86.00-157.00   50
  6  \w    -20.00  63.00   0.50    4.66    --   49.53 -57.00 -60.00  166
  7  \w     89.00 114.00   0.50    4.66    --   54.00  76.00 -50.99   50
  8  \w     33.00  84.00   0.50    4.66    --   54.00  76.00 -50.99  102
  9  \w     37.00 120.00   0.50    4.66    --   54.00  70.00 176.33  166
 10  \w     87.00 112.00   0.50    4.66    --   54.00  36.00  17.03   50
 11  \w     46.00  96.00   0.50    4.66    --   54.00  47.00  60.14  100
 12  \w    136.00 164.00   0.50    4.66    --   99.84  77.00 -30.00   56
 13  \w    108.00 164.00   0.50    4.66    --   99.84 125.00-150.00  112
 14  \w     35.00 105.00   0.50    4.66    --   99.84 -99.00 150.00  140
 15  \w     79.00 160.00   0.50    4.66    --   99.84  77.00 -60.00  162
 16  \w     98.00 175.00   0.50    4.66    --   99.84  38.00 -90.00  154
 17  \w     44.00  70.00   0.50    4.66    --  105.46 -97.00-117.13   52
 18  \w     71.00 107.00   0.50    4.66    --  105.46 -48.00-171.76   72
 19  \w     47.00  94.00   0.50    4.66    --  105.46 -93.00  80.44   94
 20  \w     33.00  58.00   0.50    4.66    --  105.46 -48.00-171.76   50
 21  \w     88.00 114.00   0.50    4.66    --  105.46 -61.00 -39.27   52
 22  \w     39.00  65.00   0.50    4.66    --  105.46 -61.00 -39.27   52
;
_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_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.9963
_diffrn_reflns_Laue_measured_fraction_max 0.9486
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            48283
_diffrn_reflns_point_group_measured_fraction_full 0.9963
_diffrn_reflns_point_group_measured_fraction_max 0.9486
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.19
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.60a (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       plate
_exptl_crystal_F_000             5040.455
_exptl_crystal_recrystallization_method 'Slow evaporation from hexane'
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.5451
_refine_diff_density_min         -0.3470
_refine_diff_density_rms         0.0494
_refine_ls_d_res_high            0.7906
_refine_ls_d_res_low             11.9692
_refine_ls_goodness_of_fit_ref   1.0248
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    186
_refine_ls_number_parameters     728
_refine_ls_number_reflns         14327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0248
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+8.8752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1404
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              62
_reflns_limit_l_min              -64
_reflns_number_gt                11634
_reflns_number_total             14327
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc03904a3.cif
_cod_data_source_block           xstr1583_auto
_cod_depositor_comments
'Adding full bibliography for 7133782--7133785.cif.'
_cod_database_code               7133784
_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. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C25) = Uanis(C23) = Uanis(C20) = Uanis(C22) = Uanis(C24) =
Uanis(C21)
Uanis(C10A) = Uanis(C20A) = Uanis(C17)
Uanis(C16A) = Uanis(C15A) = Uanis(C14A) = Uanis(C13A) = Uanis(C12A) =
Uanis(C17A)
3. Others
 Sof(H5)=Sof(H3)=Sof(C74)=Sof(H74a)=Sof(H74b)=Sof(H74c)=Sof(C73)=Sof(H73a)=
 Sof(H73b)=Sof(H73c)=1-FVAR(1)
 Sof(H2)=Sof(H6)=Sof(C7)=Sof(H7a)=Sof(H7b)=Sof(H7c)=Sof(C8)=Sof(H8a)=Sof(H8b)=
 Sof(H8c)=FVAR(1)
 Sof(H17)=Sof(C20A)=Sof(H20a)=Sof(H20b)=Sof(H20c)=Sof(C10A)=Sof(H10a)=
 Sof(H10b)=Sof(H10c)=1-FVAR(2)
 Sof(H17a)=Sof(C18)=Sof(H18a)=Sof(H18b)=Sof(H18c)=Sof(C19)=Sof(H19a)=Sof(H19b)=
 Sof(H19c)=FVAR(2)
 Sof(C12A)=Sof(C17A)=Sof(H17b)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(C14A)=
 Sof(H14A)=Sof(C13A)=Sof(H13A)=Sof(C11A)=Sof(H11a)=Sof(H11b)=Sof(H11c)=1-FVAR(3)
 Sof(C26)=Sof(H26a)=Sof(H26b)=Sof(H26c)=Sof(C23)=Sof(C22)=Sof(H22)=Sof(C21)=
 Sof(H21)=Sof(C20)=Sof(C25)=Sof(H25)=Sof(C24)=Sof(H24)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C17(H17a), C17(H17), C4(H4), C1(H1), C51(H51), C48(H48), C27(H27), C70(H70),
 C36(H36), C67(H67), C39(H39)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C5(H5), C3(H3), C55(H55), C44(H44), C56(H56), C59(H59),
 C58(H58), C46(H46), C45(H45), C15(H15), C13(H13), C14(H14), C33(H33), C34(H34),
  C32(H32), C64(H64), C63(H63), C65(H65), C22(H22), C21(H21), C25(H25),
 C24(H24), C17A(H17b), C16A(H16A), C14A(H14A), C13A(H13A)
4.c Fitted hexagon refined as free rotating group:
 C23(C22,C21,C20,C25,C24), C12A(C17A,C16A,C15A,C14A,C13A)
4.d Idealised Me refined as rotating group:
 C68(H68a,H68b,H68c), C49(H49a,H49b,H49c), C69(H69a,H69b,H69c), C52(H52a,H52b,
 H52c), C50(H50a,H50b,H50c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c), C60(H60a,
 H60b,H60c), C71(H71a,H71b,H71c), C38(H38a,H38b,H38c), C37(H37a,H37b,H37c),
 C53(H53a,H53b,H53c), C72(H72a,H72b,H72c), C41(H41a,H41b,H41c), C40(H40a,H40b,
 H40c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C74(H74a,H74b,H74c), C73(H73a,H73b,
 H73c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20A(H20a,H20b,H20c),
 C10A(H10a,H10b,H10c), C26(H26a,H26b,H26c), C11A(H11a,H11b,H11c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;