Controlled hydrolysis of AlMe<sub>3</sub> to tetramethylalumoxane and a new look at incipient adducts with water.
Korona, Krzesimir; Justyniak, Iwona; Pogrebetsky, James; Lemieszka, Marta; Bernatowicz, Piotr; Pietrzykowski, Antoni; Kubas, Adam; Lewiński, Janusz; Chemical communications (Cambridge, England) 60 (2024) 9392–9395; doi:10.1039/d4cc03672g

data_7133465
_publ_section_title
;
 Controlled hydrolysis of AlMe<sub>3</sub> to tetramethylalumoxane and a
 new look at incipient adducts with water.
;
_journal_issue                   70
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9392
_journal_page_last               9395
_journal_paper_doi               10.1039/d4cc03672g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '2(C11 H22 Al2 N2 O)'
_chemical_formula_sum            'C22 H44 Al4 N4 O2'
_chemical_formula_weight         504.53
_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             2024-07-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                86.298(3)
_cell_angle_beta                 77.725(3)
_cell_angle_gamma                73.794(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1180(4)
_cell_length_b                   13.7490(6)
_cell_length_c                   14.0249(4)
_cell_measurement_reflns_used    3800
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      70.0570
_cell_measurement_theta_min      3.2330
_cell_volume                     1468.79(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.833
_diffrn_measured_fraction_theta_max 0.820
_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    -14.00  12.00   1.00    1.00    --    0.00  57.00-180.00   26
  2  \w    -26.00  21.00   1.00    1.00    --    0.00 -57.00 -60.00   47
  3  \w    -57.00 -28.00   1.00    1.00    --    0.00 -57.00 -60.00   29
  4  \w     24.00  84.00   1.00    4.00    --   54.50-125.00 -90.00   60
  5  \w     -2.00  78.00   1.00    4.00    --   54.50 -77.00 -60.00   80
  6  \w      5.00 119.00   1.00    4.00    --   54.50   0.00 -60.00  114
  7  \w     72.00 117.00   1.00    5.50    --  108.00 -50.00 -90.00   45
  8  \w    145.00 178.00   1.00    5.50    --  108.00  37.00 150.00   33
  9  \w     85.00 133.00   1.00    5.50    --  108.00 -91.00-120.00   48
 10  \w    107.00 159.00   1.00    5.50    --  108.00  37.00 -60.00   52
 11  \w     72.00 134.00   1.00    5.50    --  108.00 -25.00  60.00   62
 12  \w     41.00  71.00   1.00    5.50    --  108.00 -63.00  90.00   30
 13  \w     84.00 123.00   1.00    5.50    --  108.00 -63.00  90.00   39
 14  \w     40.00 113.00   1.00    5.50    --  108.00-111.00 120.00   73
 15  \w     83.00 114.00   1.00    5.50    --  108.00 -91.00 150.00   31
 16  \w     54.00  79.00   1.00    5.50    --  108.00-111.00  30.00   25
 17  \w     42.00  69.00   1.00    5.50    --  108.00 -91.00 150.00   27
 18  \w     59.00 101.00   1.00    5.50    --  108.00-111.00  60.00   42
 19  \w     36.00 142.00   1.00    5.50    --  108.00 -25.00   0.00  106
 20  \w     84.00 157.00   1.00    5.50    --  108.00  37.00-120.00   73
 21  \w     43.00  68.00   1.00    5.50    --  108.00 -91.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2009501000
_diffrn_orient_matrix_UB_12      -0.0388166000
_diffrn_orient_matrix_UB_13      -0.0296974000
_diffrn_orient_matrix_UB_21      0.0138490000
_diffrn_orient_matrix_UB_22      0.1095916000
_diffrn_orient_matrix_UB_23      -0.0013577000
_diffrn_orient_matrix_UB_31      0.0127225000
_diffrn_orient_matrix_UB_32      -0.0099332000
_diffrn_orient_matrix_UB_33      0.1084151000
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.833
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7000
_diffrn_reflns_point_group_measured_fraction_full 0.833
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.072
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0280P)^2^+1.9664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4102
_reflns_number_total             4558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03672g2.cif
_cod_data_source_block           comp4
_cod_depositor_comments
'Adding full bibliography for 7133464--7133465.cif.'
_cod_database_code               7133465
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H40 N4 O4 Al4'
_reflns_odcompleteness_completeness 73.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_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 Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C8(H8), C9(H9), C16(H16), C17(H17), C19(H19), C20(H20)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              31396
_shelx_hkl_checksum              68534
_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 1.638
_oxdiff_exptl_absorpt_empirical_full_min 0.609