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_7060674
_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         'C34 H52 Cl2 In N3 P2'
_chemical_formula_sum            'C34 H52 Cl2 In N3 P2'
_chemical_formula_weight         750.44
_chemical_name_systematic        'LInCl2 (Mes)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-23
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.03.16 svn.rd6aaa9fc for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-04-28 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3340(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.28430(10)
_cell_length_b                   19.1068(3)
_cell_length_c                   20.8295(3)
_cell_measurement_reflns_used    21802
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      79.3780
_cell_measurement_theta_min      4.2450
_cell_volume                     3691.95(9)
_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 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 0.999
_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    -42.00  28.00   0.50    2.09    --  -38.50  37.00 -30.00  140
  2  \w   -103.00 -15.00   0.50    2.09    --  -38.50 -77.00-150.00  176
  3  \w    -50.00  25.00   0.50    2.09    --  -38.50  57.00  60.00  150
  4  \w    -42.00  28.00   0.50    2.09    --  -38.50  37.00   0.00  140
  5  \w     23.00 100.00   0.50    2.09    --   49.06-125.00 -90.00  154
  6  \w     41.00 143.00   0.50    8.37    --  111.00 -91.00  30.00  204
  7  \w     44.00 114.00   0.50    8.37    --  111.00 -37.00-120.00  140
  8  \w     96.00 174.00   0.50    8.37    --  111.00  63.00 -30.00  156
  9  \w     47.00 117.00   0.50    8.37    --  111.00 -50.00  30.00  140
 10  \w     57.00 151.00   0.50    8.37    --  111.00 178.00   0.00  188
 11  \w     47.00 117.00   0.50    8.37    --  111.00 -50.00  60.00  140
 12  \w    105.00 175.00   0.50    8.37    --  111.00  50.00-180.00  140
 13  \w     44.00 114.00   0.50    8.37    --  111.00 -37.00  60.00  140
 14  \w     41.00 115.00   0.50    8.37    --  111.00 -25.00 150.00  148
 15  \w     48.00 126.00   0.50    8.37    --  111.00 -63.00-120.00  156
 16  \w     41.00 116.00   0.50    8.37    --  111.00-111.00  30.00  150
 17  \w     41.00 115.00   0.50    8.37    --  111.00 -25.00  30.00  148
 18  \w     48.00 126.00   0.50    8.37    --  111.00 -63.00  60.00  156
 19  \w     41.00 116.00   0.50    8.37    --  111.00-111.00  90.00  150
 20  \w    101.00 178.00   0.50    8.37    --  111.00  12.00-150.00  154
 21  \w     75.00 111.00   0.50    8.37    --  111.00-111.00 120.00   72
 22  \w    115.00 165.00   0.50    8.37    --  111.00 111.00-180.00  100
 23  \w     86.00 112.00   0.50    8.37    --  111.00-111.00  60.00   52
 24  \w     52.00 104.00   0.50    8.37    --  111.00 -37.00 150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41210
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.800
_diffrn_reflns_theta_min         4.249
_exptl_absorpt_coefficient_mu    7.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73751
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       needle
_exptl_crystal_F_000             1560
_exptl_crystal_preparation       'Prepared with paratone oil'
_exptl_crystal_recrystallization_method
'Grown via slow evaporation of a solution of toluene:heptane (1:3)'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0452P)^2^+1.7245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7124
_reflns_number_total             7991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph17080
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060674
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 P004-N3 \\sim P0-N3
 with sigma of 0.02
 P004-C4 \\sim P0-C4
 with sigma of 0.02
 P004-C21 \\sim P0-C21A
 with sigma of 0.02
 P004-C24 \\sim P0-C24A
 with sigma of 0.02
 C23-C25 \\sim C23A-C25A
 with sigma of 0.04
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C21-C22 \\sim C21A-C22A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C20-C22 \\sim C20A-C22A
 with sigma of 0.04
 C24-C25 \\sim C24A-C25A
 with sigma of 0.02
 P004-C23 \\sim P0-C23A
 with sigma of 0.04
 P004-C20 \\sim P0-C20A
 with sigma of 0.04
 P004-C22 \\sim P0-C22A
 with sigma of 0.04
 P004-C25 \\sim P0-C25A
 with sigma of 0.04
 N3-C21 \\sim N3-C21A
 with sigma of 0.04
 N3-C24 \\sim N3-C24A
 with sigma of 0.04
 C4-C21 \\sim C4-C21A
 with sigma of 0.04
 C4-C24 \\sim C4-C24A
 with sigma of 0.04
 C21-C24 \\sim C21A-C24A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C21A \\sim C21: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
P004 \\sim P0: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
3. Rigid body (RIGU) restrains
 P0, C21A, C23A, C24A, C22A, C20A, C25A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P004, C24, C25, C21, C22, C23, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(P0)=Sof(C21A)=Sof(H21A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C20A)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C24A)=Sof(H24A)=Sof(C22A)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(P004)=Sof(C21)=Sof(H21)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C20)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C24)=Sof(H24)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C6(H6), C9(H9), C21(H21), C24(H24), C21A(H21A), C24A(H24A)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C2(H2), C28(H28), C3(H3), C15(H15), C30(H30)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C19(H19A,H19B,H19C), C34(H34A,H34B,
 H34C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C33(H33A,H33B,H33C), C18(H18A,H18B,
 H18C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C23(H23A,H23B,H23C), C20(H20A,
 H20B,H20C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C23A(H23D,H23E,H23F),
 C20A(H20D,H20E,H20F), C22A(H22D,H22E,H22F), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              61308
_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
;