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_7060671
_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 (Ar = Pipp)'
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-07
_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                90
_cell_angle_beta                 112.9950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.3379(2)
_cell_length_b                   23.9920(2)
_cell_length_c                   20.6103(2)
_cell_measurement_reflns_used    29222
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      79.3720
_cell_measurement_theta_min      9.0270
_cell_volume                     7436.85(14)
_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(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.942
_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    2.72    --  -38.50  37.00-180.00  140
  2  \w   -108.00 -33.00   0.50    2.72    --  -38.50 -19.00-150.00  150
  3  \w   -105.00 -35.00   0.50    2.72    --  -38.50 -37.00 150.00  140
  4  \w    -18.00  53.00   0.50    2.72    --   49.06 -37.00 120.00  142
  5  \w     41.00 116.00   0.50   10.87    --  111.00-111.00 150.00  150
  6  \w     57.00 151.00   0.50   10.87    --  111.00 178.00 -60.00  188
  7  \w     41.00 121.00   0.50   10.87    --  111.00 -12.00  60.00  160
  8  \w     46.00 134.00   0.50   10.87    --  111.00 -77.00 150.00  176
  9  \w    101.00 178.00   0.50   10.87    --  111.00  12.00  90.00  154
 10  \w    105.00 175.00   0.50   10.87    --  111.00  50.00-180.00  140
 11  \w     47.00 117.00   0.50   10.87    --  111.00 -50.00-180.00  140
 12  \w    100.00 178.00   0.50   10.87    --  111.00 111.00 -60.00  156
 13  \w     26.00 114.00   0.50    2.72    --   49.06  77.00  60.00  176
 14  \w     37.00 112.00   0.50    2.72    --   49.06  57.00 -30.00  150
 15  \w     23.00 100.00   0.50    2.72    --   49.06-125.00  30.00  154
 16  \w    105.00 130.00   0.50   10.87    --  111.00  50.00-120.00   50
;
_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      0.0336264000
_diffrn_orient_matrix_UB_12      0.0572295000
_diffrn_orient_matrix_UB_13      0.0338249000
_diffrn_orient_matrix_UB_21      -0.0385012000
_diffrn_orient_matrix_UB_22      0.0274375000
_diffrn_orient_matrix_UB_23      -0.0733936000
_diffrn_orient_matrix_UB_31      -0.0887680000
_diffrn_orient_matrix_UB_32      0.0098157000
_diffrn_orient_matrix_UB_33      0.0079867000
_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  0.0849
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            49809
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.828
_diffrn_reflns_theta_min         3.468
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79072
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       needle
_exptl_crystal_F_000             3120
_exptl_crystal_preparation       'crystal prepared with a paratone oil'
_exptl_crystal_recrystallization_method
'Crystallised by slow evaporation of a concetrated solution of toluene'
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.504
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         15266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13720
_reflns_number_total             15266
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -178.5660\% 
around [0.01 0.01 1.00] (reciprocal) or [0.46 0.00 0.89] (direct)
;
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph17078_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060671
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H52 Cl2 In N3 P2'
_chemical_oxdiff_usercomment     'Clear long needles'
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.151
_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:
 C23(H23), C5(H5), C42(H42), C39(H39), C57(H57), C51(H51), C8(H8), C20(H20),
 C54(H54), C17(H17), C32(H32), C66(H66)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C3(H3), C12(H12), C2(H2), C15(H15), C46(H46), C47(H47), C30(H30),
 C16(H16), C65(H65), C64(H64), C49(H49), C36(H36), C50(H50), C13(H13), C62(H62),
  C37(H37), C28(H28), C61(H61), C27(H27)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C44(H44A,H44B,H44C), C58(H58A,H58B,H58C), C7(H7A,H7B,
 H7C), C43(H43A,H43B,H43C), C55(H55A,H55B,H55C), C21(H21A,H21B,H21C), C40(H40A,
 H40B,H40C), C6(H6A,H6B,H6C), C25(H25A,H25B,H25C), C59(H59A,H59B,H59C),
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C41(H41A,H41B,H41C),
  C56(H56A,H56B,H56C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C), C33(H33A,H33B,
 H33C), C53(H53A,H53B,H53C), C52(H52A,H52B,H52C), C18(H18A,H18B,H18C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              79708
_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 1.475
_oxdiff_exptl_absorpt_empirical_full_min 0.527
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2