Synthesis and characterization of group 13 dichloride (M = Ga, In), dimethyl (M = Al) and cationic methyl aluminum complexes supported by monoanionic NNN-pincer ligands
Chisholm, Desmond T.; Hayes, Paul G.; New Journal of Chemistry 45 (2021) 15043–15052; doi:10.1039/D1NJ01064F

data_7060673
_publ_section_title
;
 Synthesis and characterization of group 13 dichloride (M = Ga, In),
 dimethyl (M = Al) and cationic methyl aluminum complexes supported by
 monoanionic NNN-pincer ligands
;
_journal_issue                   33
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15043
_journal_page_last               15052
_journal_paper_doi               10.1039/D1NJ01064F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C36 H58 Al N3 P2'
_chemical_formula_sum            'C36 H58 Al N3 P2'
_chemical_formula_weight         621.77
_chemical_name_systematic        'LAlMe2 (Ar = Mes)'
_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             2021-04-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-28 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                66.419(2)
_cell_angle_beta                 82.147(3)
_cell_angle_gamma                77.448(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5179(4)
_cell_length_b                   14.3557(4)
_cell_length_c                   16.0481(4)
_cell_measurement_reflns_used    16735
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      79.0710
_cell_measurement_theta_min      3.5890
_cell_volume                     1752.81(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.72a (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      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.950
_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   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00  30.00  176
  2  \w    -44.00  31.00   0.50    0.50    --  -38.50  19.00 120.00  150
  3  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00 -60.00  176
  4  \w   -102.00 -27.00   0.50    0.50    --  -38.50 -57.00-180.00  150
  5  \w    -90.00  -2.00   0.50    0.50    --  -38.50 125.00-150.00  176
  6  \w    -42.00  28.00   0.50    0.50    --  -38.50  37.00-180.00  140
  7  \w     45.00 115.00   0.50    0.50    --   48.81  37.00-150.00  140
  8  \w    -14.00  61.00   0.50    0.50    --   48.81 -57.00  60.00  150
  9  \w     45.00 115.00   0.50    0.50    --   48.81  37.00  30.00  140
 10  \w     41.00 115.00   0.50    1.86    --  111.00 -25.00 -90.00  148
 11  \w     41.00 115.00   0.50    1.86    --  111.00 -25.00  90.00  148
 12  \w     44.00 114.00   0.50    1.86    --  111.00 -37.00-180.00  140
 13  \w     41.00 115.00   0.50    1.86    --  111.00 -25.00   0.00  148
 14  \w     41.00 116.00   0.50    1.86    --  111.00-111.00  30.00  150
 15  \w     41.00 116.00   0.50    1.86    --  111.00-111.00 -30.00  150
 16  \w     48.00 126.00   0.50    1.86    --  111.00 -63.00  90.00  156
 17  \w     41.00 143.00   0.50    1.86    --  111.00 -91.00  90.00  204
 18  \w     47.00 117.00   0.50    1.86    --  111.00 -50.00  60.00  140
 19  \w     41.00 115.00   0.50    1.86    --  111.00 -25.00-150.00  148
 20  \w     41.00 116.00   0.50    1.86    --  111.00-111.00-150.00  150
 21  \w     48.00 126.00   0.50    1.86    --  111.00 -63.00-120.00  156
 22  \w    101.00 178.00   0.50    1.86    --  111.00  12.00  30.00  154
 23  \w     41.00 116.00   0.50    1.86    --  111.00-111.00  90.00  150
 24  \w     48.00 126.00   0.50    1.86    --  111.00 -63.00 150.00  156
 25  \w     41.00 121.00   0.50    1.86    --  111.00 -12.00 150.00  160
 26  \w    101.00 178.00   0.50    1.86    --  111.00  12.00 -90.00  154
 27  \w     41.00 143.00   0.50    1.86    --  111.00 -91.00-120.00  204
 28  \w     41.00 143.00   0.50    1.86    --  111.00 -91.00 -90.00  204
 29  \w    107.00 178.00   0.50    1.86    --  111.00  25.00 150.00  142
 30  \w     44.00 114.00   0.50    1.86    --  111.00 -37.00 -60.00  140
 31  \w     41.00 115.00   0.50    1.86    --  111.00 -25.00 120.00  148
 32  \w     41.00 116.00   0.50    1.86    --  111.00-111.00 150.00  150
 33  \w     46.00 134.00   0.50    1.86    --  111.00 -77.00   0.00  176
 34  \w     41.00 116.00   0.50    1.86    --  111.00-111.00-120.00  150
 35  \w    107.00 178.00   0.50    1.86    --  111.00  25.00  60.00  142
 36  \w     48.00 126.00   0.50    1.86    --  111.00 -63.00 -60.00  156
 37  \w    105.00 175.00   0.50    1.86    --  111.00  50.00  60.00  140
 38  \w    101.00 178.00   0.50    1.86    --  111.00  12.00 150.00  154
 39  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00 -30.00  150
 40  \w   -103.00 -15.00   0.50    0.50    --  -38.50 -77.00 120.00  176
 41  \w     25.00 113.00   0.50    0.50    --   48.81  77.00-180.00  176
 42  \w     25.00 113.00   0.50    0.50    --   48.81  77.00 -60.00  176
 43  \w     25.00 113.00   0.50    0.50    --   48.81  77.00-120.00  176
 44  \w     25.00 113.00   0.50    0.50    --   48.81  77.00  90.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141192000
_diffrn_orient_matrix_UB_12      -0.1050803000
_diffrn_orient_matrix_UB_13      0.0809398000
_diffrn_orient_matrix_UB_21      -0.0904706000
_diffrn_orient_matrix_UB_22      0.0538729000
_diffrn_orient_matrix_UB_23      0.0631417000
_diffrn_orient_matrix_UB_31      -0.1614149000
_diffrn_orient_matrix_UB_32      -0.0148693000
_diffrn_orient_matrix_UB_33      -0.0216108000
_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  0.0749
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33604
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.719
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       plate
_exptl_crystal_F_000             676
_exptl_crystal_preparation       'Crystal was prepared with Paratone'
_exptl_crystal_recrystallization_method
'Crystals were grown from a concetrated solution of 1:3 Toluene:Pentane'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1162P)^2^+2.3985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6205
_reflns_number_total             7267
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.8806\% 
around [0.82 0.41 0.40] (reciprocal) or [1.00 0.02 0.06] (direct)
;
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph17054_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060673
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H58 Al N3 P2 '
_chemical_oxdiff_usercomment     'Clear block '
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.714
_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:
 C00B(H00B), C00I(H00I), C00L(H00L), C00V(H00)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00K(H00K), C00P(H00S), C00S(H00Z), C010(H010)
2.c Idealised Me refined as rotating group:
 C00G(H00A,H00E,H00F), C00J(H00G,H00H,H00J), C00N(H00M,H00N,H00O), C00O(H00P,
 H00Q,H00R), C00Q(H00T,H00U,H00V), C00R(H00W,H00X,H00Y), C00W(H1,H,HA), C00X(H2,
 HB,HC), C00Y(H3,HD,HE), C00Z(H4,HF,HG), C011(H01A,H01B,H01C), C012(H01D,H01E,
 H01F), C013(H01G,H01H,H01I), C014(H01J,H01K,H01L), C015(H01M,H01N,H01O),
 C016(H01P,H01Q,H01R)
;
_shelx_res_checksum              59749
_olex2_exptl_crystal_mounting_method 'Mounted on a MiTeGen Loop at 100 K'
_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 1.253
_oxdiff_exptl_absorpt_empirical_full_min 0.790
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2