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_7060676
_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         'C40 H64 Cl2 Ga N3 P2, C3 H3'
_chemical_formula_sum            'C43 H67 Cl2 Ga N3 P2'
_chemical_formula_weight         828.55
_chemical_name_systematic        'LGaCl2 (Dipp)'
_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             2021-03-01
_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                 99.4290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.50090(10)
_cell_length_b                   18.34940(10)
_cell_length_c                   25.5029(2)
_cell_measurement_reflns_used    42634
_cell_measurement_temperature    100.01(13)
_cell_measurement_theta_max      79.4720
_cell_measurement_theta_min      4.2490
_cell_volume                     4386.00(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      100.01(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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    0.50    --  -38.50  38.00-180.00  140
  2  \w   -105.00 -35.00   0.50    0.50    --  -38.50 -38.00 150.00  140
  3  \w    -42.00  28.00   0.50    0.50    --  -38.50  36.00 110.00  140
  4  \w   -102.00 -27.00   0.50    0.50    --  -38.50 -57.00 -60.00  150
  5  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00-120.00  150
  6  \w    105.00 175.00   0.50    0.58    --  111.00  50.00-150.00  140
  7  \w     88.00 176.00   0.50    0.58    --  111.00  77.00-120.00  176
  8  \w     41.00 141.00   0.50    0.58    --  111.00 -89.00 128.00  200
  9  \w     48.00 126.00   0.50    0.58    --  111.00 -63.00 120.00  156
 10  \w    107.00 178.00   0.50    0.58    --  111.00  25.00-180.00  142
 11  \w    107.00 177.00   0.50    0.58    --  111.00  38.00   0.00  140
 12  \w     45.00 115.00   0.50    0.58    --  111.00 -38.00  90.00  140
 13  \w     41.00 121.00   0.50    0.58    --  111.00 -12.00-120.00  160
 14  \w    107.00 177.00   0.50    0.58    --  111.00  38.00  30.00  140
 15  \w    100.00 178.00   0.50    0.58    --  111.00 111.00-180.00  156
 16  \w     47.00 117.00   0.50    0.58    --  111.00 -50.00-180.00  140
 17  \w    100.00 178.00   0.50    0.58    --  111.00 111.00-150.00  156
 18  \w    -16.00  73.00   0.50    0.50    --   49.06 -77.00 -30.00  178
 19  \w     26.00 114.00   0.50    0.50    --   49.06  77.00-150.00  176
 20  \w     26.00 114.00   0.50    0.50    --   49.06  77.00  90.00  176
 21  \w     37.00 112.00   0.50    0.50    --   49.06  57.00   0.00  150
 22  \w    107.00 178.00   0.50    0.58    --  111.00  25.00  90.00  142
 23  \w     41.00 116.00   0.50    0.58    --  111.00-111.00   0.00  150
 24  \w    107.00 178.00   0.50    0.58    --  111.00  25.00 -60.00  142
 25  \w    107.00 178.00   0.50    0.58    --  111.00  25.00 -30.00  142
 26  \w     41.00 116.00   0.50    0.58    --  111.00-111.00  60.00  150
 27  \w     88.00 126.00   0.50    0.58    --  111.00  77.00  60.00   76
 28  \w     88.00 176.00   0.50    0.58    --  111.00  77.00 120.00  176
;
_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      0.0412839000
_diffrn_orient_matrix_UB_12      -0.0755109000
_diffrn_orient_matrix_UB_13      0.0240107000
_diffrn_orient_matrix_UB_21      -0.1498840000
_diffrn_orient_matrix_UB_22      -0.0080407000
_diffrn_orient_matrix_UB_23      0.0150219000
_diffrn_orient_matrix_UB_31      -0.0534218000
_diffrn_orient_matrix_UB_32      -0.0357611000
_diffrn_orient_matrix_UB_33      -0.0542890000
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            59393
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.813
_diffrn_reflns_theta_min         3.514
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_exptl_crystal_preparation       'Prepared using paratone oil'
_exptl_crystal_recrystallization_method 'crystallised from benzene'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         9471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+3.0417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8755
_reflns_number_total             9471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph16061
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060676
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H64 Cl2 Ga N3 P2'
_chemical_oxdiff_usercomment     'Large clear block'
_shelx_estimated_absorpt_t_max   0.822
_shelx_estimated_absorpt_t_min   0.457
_reflns_odcompleteness_completeness 99.83
_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:
 C21(H21), C9(H9), C27(H27), C39(H39), C6(H6), C36(H36), C18(H18), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C3(H3), C2(H2), C32(H32), C13(H13), C31(H31), C15(H15), C14(H14),
 C01D(H01D), C01E(H01E), C01F(H01F)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C19(H19A,H19B,
 H19C), C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C38(H38A,
 H38B,H38C), C5(H5A,H5B,H5C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C),
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C17(H17A,H17B,H17C), C35(H35A,H35B,
 H35C), C40(H40A,H40B,H40C)
;
_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 1.462
_oxdiff_exptl_absorpt_empirical_full_min 0.733