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_7060675
_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 (Pipp)'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-01 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.9810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2460(2)
_cell_length_b                   24.0391(2)
_cell_length_c                   20.6349(3)
_cell_measurement_reflns_used    31769
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      79.5890
_cell_measurement_theta_min      3.4740
_cell_volume                     7419.15(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.945
_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    -50.00  25.00   0.50    1.56    --  -38.50  57.00-120.00  150
  2  \w    -42.00  28.00   0.50    1.56    --  -38.50  37.00 120.00  140
  3  \w    -21.00  55.00   0.50    1.56    --   49.06 -19.00 -30.00  152
  4  \w    -18.00  53.00   0.50    1.56    --   49.06 -37.00 -60.00  142
  5  \w     44.00 114.00   0.50    6.25    --  111.00 -37.00 -60.00  140
  6  \w    100.00 178.00   0.50    6.25    --  111.00 111.00 -60.00  156
  7  \w     41.00 116.00   0.50    6.25    --  111.00-111.00 -60.00  150
  8  \w     41.00 116.00   0.50    6.25    --  111.00-111.00 -30.00  150
  9  \w    107.00 178.00   0.50    6.25    --  111.00  25.00-120.00  142
 10  \w    105.00 175.00   0.50    6.25    --  111.00  50.00-150.00  140
 11  \w     47.00 117.00   0.50    6.25    --  111.00 -50.00 -60.00  140
 12  \w     52.00  97.00   0.50    6.25    --  111.00 -50.00 150.00   90
 13  \w     70.00  96.00   0.50    6.25    --  111.00 -50.00-150.00   52
 14  \w    101.00 167.00   0.50    6.25    --  111.00  12.00 -30.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0771254000
_diffrn_orient_matrix_UB_12      -0.0101177000
_diffrn_orient_matrix_UB_13      -0.0717778000
_diffrn_orient_matrix_UB_21      0.0183097000
_diffrn_orient_matrix_UB_22      -0.0630239000
_diffrn_orient_matrix_UB_23      0.0081304000
_diffrn_orient_matrix_UB_31      -0.0657527000
_diffrn_orient_matrix_UB_32      -0.0057413000
_diffrn_orient_matrix_UB_33      0.0368596000
_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  0.0273
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45166
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.936
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_preparation       'Crystal with paratone oil'
_exptl_crystal_recrystallization_method
'crystal grown by slow evaporation from a solution of toluene:heptane (1:2)'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     785
_refine_ls_number_reflns         15306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0546P)^2^+6.2641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13705
_reflns_number_total             15306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph17042
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060675
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H70 Al N3 P2'
_chemical_oxdiff_usercomment     'Medium clear crystal'
_shelx_estimated_absorpt_t_max   0.916
_shelx_estimated_absorpt_t_min   0.830
_reflns_odcompleteness_completeness 95.84
_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 Ternary CH refined with riding coordinates:
 C00D(H00D), C013(H013), C014(H014), C01A(H01X), C01B(H01B), C01E(H01E),
 C01G(H01G), C01J(H01), C01L(H2), C01Q(H01Q), C01U(H7), C01Z(H01Z)
2.b Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00I(H00I), C00L(H00L), C00M(H00M), C00O(H00O),
 C00Q(H00Q), C00T(H00T), C00V(H00V), C00Y(H00Y), C00Z(H00Z), C010(H010),
 C011(H011), C012(H012), C015(H015), C017(H017), C01F(H01F), C01H(H01Y),
 C01K(H1), C01O(H4)
2.c Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C016(H01R,H01S,H01T), C019(H01U,H01V,H01W), C1(H1A,H1B,
 H1C), C01I(H01A,H01C,H01D), C01M(H3,H,HA), C01N(H01H,H01I,H01J), C2(H2A,H2B,
 H2C), C01R(H5,HB,HC), C01S(H01K,H01L,H01M), C01T(H6,HD,HE), C01V(H01N,H01O,
 H01P), C01W(H8,HF,HG), C01X(H9,HH,HI), C01Y(H10,HJ,HK), C020(H02A,H02B,H02C),
 C021(H02D,H02E,H02F), C022(H02G,H02H,H02I), C023(H02V,H02W,H02X), C024(H02J,
 H02K,H02L), C025(H02M,H02N,H02O), C026(H02Y,HL,HM), C027(H02P,H02Q,H02R),
 C028(H02Z,HN,HO), C029(H02,HP,HQ), C02A(H02S,H02T,H02U), C02B(H11,HR,HS),
 C02C(H12,HT,HU)
;
_olex2_exptl_crystal_mounting_method 'Mounted on a MiTeGen spoon 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 1.394
_oxdiff_exptl_absorpt_empirical_full_min 0.867