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_7133464
_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         'C18 H34 Al4 N2 O2'
_chemical_formula_sum            'C18 H34 Al4 N2 O2'
_chemical_formula_weight         418.39
_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             2024-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-04-29 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                99.654(3)
_cell_angle_beta                 111.823(3)
_cell_angle_gamma                91.082(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3590(3)
_cell_length_b                   8.9229(3)
_cell_length_c                   9.2090(3)
_cell_measurement_reflns_used    3041
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      69.9140
_cell_measurement_theta_min      5.0340
_cell_volume                     626.13(4)
_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 2014/5 (Sheldrick, 2014)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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      5.00  46.82   0.82    1.00    --    0.00  57.00   0.00   51
  2  \w    -68.00 -41.76   0.82    1.00    --    0.00 -37.00-150.00   32
  3  \w    -28.00  -0.94   0.82    1.00    --    0.00 -37.00-150.00   33
  4  \w     57.00 125.88   0.82    1.50    --   54.54  37.00 -30.00   84
  5  \w     31.00  62.16   0.82    1.50    --   54.54-125.00  30.00   38
  6  \w    -14.00  75.38   0.82    1.50    --   54.54 -57.00  60.00  109
  7  \w      3.00  45.64   0.82    1.50    --   54.54 -99.00  60.00   52
  8  \w     35.00 112.90   0.82    1.50    --   54.54  57.00 -90.00   95
  9  \w     28.00 121.48   0.82    1.50    --   54.54  77.00-180.00  114
 10  \w     69.00 108.36   0.82    1.50    --   54.54-125.00-150.00   48
 11  \w     49.00  94.92   0.82    5.00    --  108.00 -25.00  30.00   56
 12  \w     87.00 175.56   0.82    5.00    --  108.00  63.00-150.00  108
 13  \w     46.00  72.24   0.82    5.00    --  108.00-111.00 150.00   32
 14  \w     68.00 117.20   0.82    5.00    --  108.00 -25.00-150.00   60
 15  \w     84.00 110.24   0.82    5.00    --  108.00-111.00  90.00   32
 16  \w     37.00 111.62   0.82    5.00    --  108.00-111.00 -90.00   91
 17  \w    102.00 136.44   0.82    5.00    --  108.00 -91.00-150.00   42
 18  \w     53.00  97.28   0.82    5.00    --  108.00 -50.00-180.00   54
 19  \w     87.00 164.90   0.82    5.00    --  108.00  63.00 150.00   95
 20  \w     37.00  63.24   0.82    5.00    --  108.00 -91.00-150.00   32
 21  \w     78.00 110.80   0.82    5.00    --  108.00-111.00   0.00   40
 22  \w     40.00  77.72   0.82    5.00    --  108.00-111.00  90.00   46
 23  \w     97.00 139.64   0.82    5.00    --  108.00  63.00-180.00   52
 24  \w     36.00  85.20   0.82    5.00    --  108.00 -91.00-180.00   60
 25  \w    100.00 126.24   0.82    5.00    --  108.00 -50.00 -90.00   32
 26  \w     86.00 111.42   0.82    5.00    --  108.00-111.00-150.00   31
 27  \w     89.00 120.98   0.82    5.00    --  108.00  63.00 -30.00   39
 28  \w    141.00 166.42   0.82    5.00    --  108.00  63.00 -30.00   31
 29  \w    118.00 149.98   0.82    5.00    --  108.00  63.00 -60.00   39
 30  \w    100.00 163.14   0.82    5.00    --  108.00 -12.00 120.00   77
 31  \w     97.00 156.04   0.82    5.00    --  108.00  50.00  30.00   72
 32  \w     93.00 118.42   0.82    5.00    --  108.00 -63.00 -60.00   31
 33  \w     38.00  86.38   0.82    5.00    --  108.00-111.00  30.00   59
 34  \w     44.00 103.04   0.82    5.00    --  108.00 -37.00-150.00   72
 35  \w     95.00 135.18   0.82    5.00    --  108.00 -77.00  60.00   49
 36  \w     92.00 117.42   0.82    5.00    --  108.00 -77.00-150.00   31
 37  \w     56.00  91.26   0.82    5.00    --  108.00 -77.00  60.00   43
;
_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      0.0240136000
_diffrn_orient_matrix_UB_12      0.0856135000
_diffrn_orient_matrix_UB_13      0.1675551000
_diffrn_orient_matrix_UB_21      -0.1881560000
_diffrn_orient_matrix_UB_22      -0.0525486000
_diffrn_orient_matrix_UB_23      -0.0303044000
_diffrn_orient_matrix_UB_31      0.0612101000
_diffrn_orient_matrix_UB_32      -0.1443061000
_diffrn_orient_matrix_UB_33      0.0683584000
_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  0.0196
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.952
_diffrn_reflns_theta_min         5.048
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.785
_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    1.110
_exptl_crystal_description       plate
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0599P)^2^+0.1783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2299
_reflns_number_total             2348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03672g2.cif
_cod_data_source_block           SHELXL_3
_cod_depositor_comments
'Adding full bibliography for 7133464--7133465.cif.'
_cod_database_code               7133464
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H30 O4 Al3'
_reflns_odcompleteness_completeness 84.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_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), C7(H7), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              39580
_shelx_hkl_checksum              91674
_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 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.533