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_7133785
_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         'C71 H90 Al2 N4, 0.25[C6H14]'
_chemical_formula_sum            'C72.5 H93.5 Al2 N4'
_chemical_formula_weight         1075.040
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_Int_Tables_number      14
_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                 105.824(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2755(2)
_cell_length_b                   20.2100(2)
_cell_length_c                   24.2085(3)
_cell_measurement_reflns_used    18697
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.2440
_cell_measurement_theta_min      3.7150
_cell_volume                     7190.38(15)
_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 0.9976
_diffrn_measured_fraction_theta_max 0.9438
_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     31.00  75.00   0.50    9.34    --   49.53  23.00 -17.00   88
  2  \w      4.00  30.00   0.50    9.34    --   49.53 -23.00 177.00   52
  3  \w     84.00 152.00   0.50    9.34    --   99.84  23.00 -17.00  136
  4  \w     62.00 101.00   0.50    9.34    --   99.84 -23.00 177.00   78
  5  \w     47.00  76.00   0.50    9.34    --   49.53-125.00-180.00   58
  6  \w     33.00  58.00   0.50    9.34    --   49.53 -38.00 -60.00   50
  7  \w     36.00 120.00   0.50    9.34    --   54.00  71.00 141.52  168
  8  \w     59.00 126.00   0.50    9.34    --   54.00  44.00 125.58  134
  9  \w     80.00 117.00   0.50    9.34    --   54.00  66.00 -64.08   74
 10  \w     41.00 116.00   0.50    9.34    --   54.00  54.00  77.12  150
 11  \w     39.00  76.00   0.50    9.34    --   54.00  66.00 -64.08   74
 12  \w     95.00 135.00   0.50    9.34    --   70.00  71.00-166.37   80
 13  \w     53.00  85.00   0.50    9.34    --   70.00  71.00-166.37   64
 14  \w     30.00 114.00   0.50    9.34    --   99.84 -57.00-150.00  168
 15  \w     37.00 106.00   0.50    9.34    --   99.84 -99.00   0.00  138
 16  \w     34.00  96.00   0.50    9.34    --   99.84-125.00 -90.00  124
 17  \w     73.00 106.00   0.50    9.34    --   99.84 -99.00 -90.00   66
 18  \w    114.00 168.00   0.50    9.34    --  105.46  78.00 -35.88  108
 19  \w     48.00  93.00   0.50    9.34    --  105.46 -94.00  46.52   90
 20  \w     72.00 107.00   0.50    9.34    --  105.46 -49.00  95.15   70
;
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.9976
_diffrn_reflns_Laue_measured_fraction_max 0.9438
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49375
_diffrn_reflns_point_group_measured_fraction_full 0.9976
_diffrn_reflns_point_group_measured_fraction_max 0.9438
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.03
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.281
_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            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_description       plate
_exptl_crystal_F_000             2337.806
_exptl_crystal_recrystallization_method 'Slow evaporation from hexane'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.3973
_refine_diff_density_min         -0.3376
_refine_diff_density_rms         0.0487
_refine_ls_d_res_high            0.7911
_refine_ls_d_res_low             11.8861
_refine_ls_goodness_of_fit_ref   1.0093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    163
_refine_ls_number_parameters     783
_refine_ls_number_reflns         14362
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.0072
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+1.6329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1336
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -19
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              -13
_reflns_number_gt                11050
_reflns_number_total             14362
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cc03904a3.cif
_cod_data_source_block           xstr1574_auto
_cod_depositor_comments
'Adding full bibliography for 7133782--7133785.cif.'
_cod_database_code               7133785
_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. Restrained distances
 C5-C6 \\sim C2-C3
 with sigma of 0.04
 C8-C22 \\sim C8-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C22-C27 \\sim C22A-C27A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C27-C26 \\sim C27A-C26A
 with sigma of 0.02
 C26-C25 \\sim C26A-C25A
 with sigma of 0.02
 C24-C25 \\sim C24A-C25A
 with sigma of 0.02
 C25-C28 \\sim C25A-C28A
 with sigma of 0.02
 C8-C23 \\sim C8-C23A
 with sigma of 0.04
 C8-C27 \\sim C8-C27A
 with sigma of 0.04
 C22-C26 \\sim C22A-C26A
 with sigma of 0.04
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C23-C27 \\sim C23A-C27A
 with sigma of 0.04
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C27-C25 \\sim C27A-C25A
 with sigma of 0.04
 C26-C24 \\sim C26A-C24A
 with sigma of 0.04
 C26-C28 \\sim C26A-C28A
 with sigma of 0.04
 C24-C28 \\sim C24A-C28A
 with sigma of 0.04
 C25A-C26A \\sim C27A-C22A \\sim C23A-C24A
 with sigma of 0.04
 C22A-C27A \\sim C26A-C25A \\sim C24A-C23A
 with sigma of 0.02
 C7-C3 \\sim C7A-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C5 \\sim C6 \\sim C2 \\sim C3: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C25A) = Uanis(C28A)
4. Others
 Sof(C22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28d)=Sof(H28e)=Sof(H28f)=1-FVAR(1)
 Sof(C22)=Sof(C23)=Sof(H23)=Sof(C27)=Sof(H27)=Sof(C26)=Sof(H26)=Sof(C24)=
 Sof(H24)=Sof(C25)=Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(H28c)=FVAR(1)
 Sof(H3)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=Sof(H7Ac)=1-FVAR(2)
 Sof(H2)=Sof(C7)=Sof(H7a)=Sof(H7b)=Sof(H7c)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C16(H16), C50(H50), C69(H69), C47(H47), C66(H66), C35(H35), C38(H38), C1(H1),
 C4(H4), C19(H19)
5.b Aromatic/amide H refined with riding coordinates:
 C58(H58), C54(H54), C57(H57), C55(H55), C45(H45), C64(H64), C62(H62),
 C12(H12), C63(H63), C43(H43), C13(H13), C14(H14), C31(H31), C44(H44), C33(H33),
  C32(H32), C5(H5), C6(H6), C2(H2), C3(H3), C23(H23), C27(H27), C26(H26),
 C24(H24), C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A)
5.c Idealised Me refined as rotating group:
 C70(H70a,H70b,H70c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C71(H71a,H71b,
 H71c), C52(H52a,H52b,H52c), C67(H67a,H67b,H67c), C51(H51a,H51b,H51c), C59(H59a,
 H59b,H59c), C37(H37a,H37b,H37c), C68(H68a,H68b,H68c), C48(H48a,H48b,H48c),
 C36(H36a,H36b,H36c), C49(H49a,H49b,H49c), C40(H40a,H40b,H40c), C39(H39a,H39b,
 H39c), C7(H7a,H7b,H7c), C28(H28a,H28b,H28c), C28A(H28d,H28e,H28f), C20(H20a,
 H20b,H20c), C21(H21a,H21b,H21c), C7A(H7Aa,H7Ab,H7Ac)
;
_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
;