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_7060670
_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 H65 N3 P2'
_chemical_formula_sum            'C40 H65 N3 P2'
_chemical_formula_weight         649.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-08 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1046(3)
_cell_length_b                   8.30160(10)
_cell_length_c                   26.1934(4)
_cell_measurement_reflns_used    11513
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      78.3830
_cell_measurement_theta_min      4.8190
_cell_volume                     3936.79(10)
_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(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_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   19.73    --  -38.50  38.00 -60.00  140
  2  \w    -50.00  25.00   0.50   19.73    --  -38.50  57.00 -30.00  150
  3  \w    -44.00  31.00   0.50   19.73    --  -38.50  19.00-120.00  150
  4  \w     43.00 119.00   0.50   19.73    --   49.06  19.00  60.00  152
  5  \w     45.00 115.00   0.50   78.91    --  111.00 -38.00  30.00  140
  6  \w     41.00 115.00   0.50   78.91    --  111.00 -25.00   0.00  148
  7  \w    107.00 177.00   0.50   78.91    --  111.00  38.00  30.00  140
  8  \w    100.00 178.00   0.50   78.91    --  111.00 111.00 -30.00  156
  9  \w     48.00 117.00   0.50   78.91    --  111.00 -63.00 -30.00  138
 10  \w     62.00 107.00   0.50   78.91    --  111.00 -25.00-150.00   90
 11  \w     47.00 112.00   0.50   78.91    --  111.00 -76.00 114.00  130
 12  \w    108.00 152.00   0.50   78.91    --  111.00  50.00-180.00   88
 13  \w     66.00 134.00   0.50   78.91    --  111.00 -77.00-120.00  136
 14  \w     61.00 117.00   0.50   78.91    --  111.00 -50.00  90.00  112
 15  \w     60.00 103.00   0.50   78.91    --  111.00 178.00  60.00   86
;
_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      -0.0466759000
_diffrn_orient_matrix_UB_12      0.1542915000
_diffrn_orient_matrix_UB_13      -0.0052570000
_diffrn_orient_matrix_UB_21      -0.0164254000
_diffrn_orient_matrix_UB_22      -0.0040507000
_diffrn_orient_matrix_UB_23      0.0577201000
_diffrn_orient_matrix_UB_31      0.0693051000
_diffrn_orient_matrix_UB_32      0.1029853000
_diffrn_orient_matrix_UB_33      0.0101220000
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22962
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.739
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94616
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.15(2)
_refine_ls_extinction_coef       0.00034(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         7740
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0516P)^2^+0.5311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.865
_reflns_Friedel_fraction_max     0.809
_reflns_number_gt                6874
_reflns_number_total             7740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph16031i
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060670
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H65N3P2
_chemical_oxdiff_usercomment     'very small clear crystal'
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.903
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.85(2)
 0.15(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8), C11(H11), C14(H14), C23(H23), C26(H26), C35(H35), C38(H38)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C19(H19), C20(H20), C21(H21), C31(H31), C32(H32), C33(H33)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              19070
_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 1.836
_oxdiff_exptl_absorpt_empirical_full_min 0.843