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_7060672
_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 H53 N3 P2, C6 H6'
_chemical_formula_sum            'C40 H59 N3 P2'
_chemical_formula_weight         643.84
_chemical_name_systematic        LMes
_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             2021-03-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-02 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.5960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6933(2)
_cell_length_b                   22.3999(3)
_cell_length_c                   14.5398(2)
_cell_measurement_reflns_used    11428
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      79.2690
_cell_measurement_theta_min      3.6260
_cell_volume                     3774.97(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 0.999
_diffrn_measured_fraction_theta_max 0.977
_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    1.53    --  -38.50  38.00-120.00  140
  2  \w   -108.00 -33.00   0.50    1.53    --  -38.50 -19.00 -60.00  150
  3  \w    -50.00  25.00   0.50    1.53    --  -38.50  57.00  60.00  150
  4  \w   -105.00 -35.00   0.50    1.53    --  -38.50 -38.00 -90.00  140
  5  \w    105.00 175.00   0.50    6.13    --  111.00  50.00 -60.00  140
  6  \w     48.00 126.00   0.50    6.13    --  111.00 -63.00  90.00  156
  7  \w     45.00 115.00   0.50    6.13    --  111.00 -38.00 -60.00  140
  8  \w    107.00 177.00   0.50    6.13    --  111.00  38.00   0.00  140
  9  \w     47.00 117.00   0.50    6.13    --  111.00 -50.00 150.00  140
 10  \w    107.00 177.00   0.50    6.13    --  111.00  38.00 -90.00  140
 11  \w     45.00 115.00   0.50    6.13    --  111.00 -38.00 150.00  140
 12  \w     52.00 116.00   0.50    6.13    --  111.00 -50.00 -90.00  128
 13  \w     49.00 122.00   0.50    6.13    --  111.00 -77.00 -90.00  146
 14  \w    115.00 170.00   0.50    6.13    --  111.00  25.00-120.00  110
 15  \w    105.00 169.00   0.50    6.13    --  111.00  50.00 -30.00  128
;
_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      -0.0148869000
_diffrn_orient_matrix_UB_12      0.0477816000
_diffrn_orient_matrix_UB_13      0.0736794000
_diffrn_orient_matrix_UB_21      0.1276343000
_diffrn_orient_matrix_UB_22      0.0176446000
_diffrn_orient_matrix_UB_23      0.0027727000
_diffrn_orient_matrix_UB_31      -0.0341532000
_diffrn_orient_matrix_UB_32      0.0461521000
_diffrn_orient_matrix_UB_33      -0.0774616000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24117
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.733
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66735
_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    1.133
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_preparation       'Crystal prepared with paratone oil'
_exptl_crystal_recrystallization_method
'Crystallised by evaporation of a concentrated solution of benzene'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0754P)^2^+1.3642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6643
_reflns_number_total             8034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01064f2.cif
_cod_data_source_block           ph16044copy1
_cod_depositor_comments
'Adding full bibliography for 7060669--7060676.cif.'
_cod_database_code               7060672
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C34H53N3P2
_chemical_oxdiff_usercomment     'Long clear prism crystal '
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.518
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C00F(H00F), C00M(H00M), C00N(H00N), C00R(H00S)
2.b Aromatic/amide H refined with riding coordinates:
 N003(H003), C00B(H00B), C00E(H00E), C00G(H00G), C00I(H00I), C00J(H00J),
 C00L(H00L), C014(H014), C015(H015), C016(H016), C017(H017), C018(H018),
 C019(H019)
2.c Idealised Me refined as rotating group:
 C00O(H00A,H00C,H00D), C00P(H00H,H00K,H00O), C00Q(H00P,H00Q,H00R), C00T(H00T,
 H00U,H00V), C00U(H00W,H00X,H00Y), C00V(H00Z,H,HA), C00W(H00,HB,HC), C00X(H1,HD,
 HE), C00Y(H2,HF,HG), C00Z(H3,HH,HI), C010(H01A,H01B,H01C), C011(H01D,H01E,
 H01F), C012(H01G,H01H,H01I), C013(H01J,H01K,H01L)
;
_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 1.639
_oxdiff_exptl_absorpt_empirical_full_min 0.706