Novel bidentate <i>N</i>-coordinated alkylaluminum complexes: synthesis, characterization, and efficient catalysis for hydrophosphonylation.
Wei, Biao; Wang, Chaoqun; Miao, Hui; Qin, Zhibiao; Huang, Mengna; Xu, Yan; Xue, Wenhui; Yang, Shucheng; Liu, Chenxu; Bai, Cuibing; Chen, Zheng; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4185–4193; doi:10.1039/d3dt04087a

data_7715369
_publ_section_title
;
 Novel bidentate <i>N</i>-coordinated alkylaluminum complexes: synthesis,
 characterization, and efficient catalysis for hydrophosphonylation.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4185
_journal_page_last               4193
_journal_paper_doi               10.1039/d3dt04087a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H31 Al N2'
_chemical_formula_sum            'C24 H31 Al N2'
_chemical_formula_weight         374.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-12-01 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.681(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.8578(15)
_cell_length_b                   11.8686(6)
_cell_length_c                   15.7892(7)
_cell_measurement_reflns_used    5977
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3180
_cell_measurement_theta_min      2.2240
_cell_volume                     4393.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.886
_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    -12.00  13.00   0.50   15.00    --   24.18 -37.00  60.00   50
  2  \w     22.00  94.00   0.50   15.00    --   24.18-128.00   6.00  144
  3  \w     36.00  78.00   0.50   15.00    --   24.18-141.00-165.00   84
  4  \w    -54.00  21.00   0.50   15.00    --   24.18 -37.00-150.00  150
  5  \w    -66.00   2.00   0.50   15.00    --   24.18 -37.00-120.00  136
  6  \w    -70.00   3.00   0.50   15.00    --   24.18 -19.00  90.00  146
  7  \w    -60.00   5.00   0.50   15.00    --   24.18 -19.00 150.00  130
  8  \w    -63.00 -37.00   0.50   15.00    --  -23.24 128.00  80.00   52
  9  \w   -106.00 -33.00   0.50   15.00    --  -23.24 141.00-107.00  146
 10  \w     67.00 107.00   0.50   15.00    --   24.18 178.00-180.00   80
 11  \w     74.00  99.00   0.50   15.00    --   24.18 178.00 -60.00   50
 12  \w   -115.00  -8.00   0.50   15.00    --  -23.24 -19.00 -60.00  214
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0220932000
_diffrn_orient_matrix_UB_12      -0.0348133000
_diffrn_orient_matrix_UB_13      0.0098009000
_diffrn_orient_matrix_UB_21      -0.0206090000
_diffrn_orient_matrix_UB_22      0.0348480000
_diffrn_orient_matrix_UB_23      -0.0257235000
_diffrn_orient_matrix_UB_31      0.0015401000
_diffrn_orient_matrix_UB_32      -0.0338426000
_diffrn_orient_matrix_UB_33      -0.0365118000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24600
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.782
_diffrn_reflns_theta_min         2.236
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1175P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.2015
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3176
_reflns_number_total             5576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04087a2.cif
_cod_data_source_block           d31-c3
_cod_database_code               7715369
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNAl
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.986
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C15(H15), C20(H20)
1.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C16(H16A,H16B), C18(H18A,H18B), C17(H17A,H17B)
1.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C13(H13), C10(H10), C12(H12), C4(H4), C11(H11), C5(H5), C7(H7), C6(H6)
1.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C22(H22A,H22B,
 H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72576
_shelx_fab_checksum              85767
_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 5.375
_oxdiff_exptl_absorpt_empirical_full_min 0.272