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_7715372
_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         'C26 H35 Al N2'
_chemical_formula_sum            'C26 H35 Al N2'
_chemical_formula_weight         402.54
_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                 100.535(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.2371(14)
_cell_length_b                   13.1513(6)
_cell_length_c                   15.8236(7)
_cell_measurement_reflns_used    7969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5080
_cell_measurement_theta_min      2.0240
_cell_volume                     4754.1(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 1.000
_diffrn_measured_fraction_theta_max 0.913
_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    -57.00   0.00   0.50   22.00    --   24.18 -37.00  90.00  114
  2  \w     14.00  51.00   0.50   22.00    --   24.18-108.00 -16.00   74
  3  \w     39.00  91.00   0.50   22.00    --   24.18-178.00 -30.00  104
  4  \w     41.00 107.00   0.50   22.00    --   24.18-178.00 120.00  132
  5  \w     -4.00  22.00   0.50   22.00    --  -23.24 -99.00 150.00   52
  6  \w    -22.00  36.00   0.50   22.00    --  -23.24 -99.00  90.00  116
  7  \w    -56.00   0.00   0.50   22.00    --   24.18 -19.00 -60.00  112
  8  \w    -31.00   3.00   0.50   22.00    --   24.18 -19.00-120.00   68
  9  \w    -65.00  18.00   0.50   22.00    --   24.18 -37.00-150.00  166
 10  \w    -71.00 -46.00   0.50   22.00    --   24.18 -19.00-120.00   50
 11  \w    -87.00 -38.00   0.50   22.00    --  -23.24 108.00  80.00   98
 12  \w    -63.00  20.00   0.50   22.00    --   24.18 -37.00 150.00  166
 13  \w     47.00 104.00   0.50   22.00    --   24.18 178.00  90.00  114
 14  \w     82.00 107.00   0.50   22.00    --   24.18 178.00-150.00   50
;
_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      -0.0255896000
_diffrn_orient_matrix_UB_12      -0.0102338000
_diffrn_orient_matrix_UB_13      -0.0307856000
_diffrn_orient_matrix_UB_21      -0.0160309000
_diffrn_orient_matrix_UB_22      0.0346211000
_diffrn_orient_matrix_UB_23      0.0211378000
_diffrn_orient_matrix_UB_31      0.0072542000
_diffrn_orient_matrix_UB_32      0.0401141000
_diffrn_orient_matrix_UB_33      -0.0261055000
_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  0.0593
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29338
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.605
_diffrn_reflns_theta_min         2.117
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53227
_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    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         6114
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0923P)^2^+0.9724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1627
_refine_ls_wR_factor_ref         0.1787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4041
_reflns_number_total             6114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04087a2.cif
_cod_data_source_block           d31-c6
_cod_database_code               7715372
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNAl
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.987
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Rigid body (RIGU) restrains
 C25, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3.a Ternary CH refined with riding coordinates:
 C15(H15), C20(H20)
3.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C25(H25A,
 H25B), C23(H23A,H23B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C13(H13), C4(H4), C7(H7), C10(H10), C12(H12), C6(H6), C5(H5), C11(H11)
3.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64890
_shelx_fab_checksum              26238
_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 3.501
_oxdiff_exptl_absorpt_empirical_full_min 0.373