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_7715370
_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         'C23 H23 Al N2'
_chemical_formula_sum            'C23 H23 Al N2'
_chemical_formula_weight         354.41
_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
_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                 90.965(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9561(5)
_cell_length_b                   14.6783(8)
_cell_length_c                   14.9503(8)
_cell_measurement_reflns_used    3544
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4590
_cell_measurement_theta_min      2.6610
_cell_volume                     1965.09(19)
_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_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0950
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12566
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.566
_diffrn_reflns_theta_min         1.944
_exptl_absorpt_coefficient_mu    0.111
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1556P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2642
_reflns_number_total             4758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04087a2.cif
_cod_data_source_block           exp_222
_cod_database_code               7715370
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.985
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B)
1.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C14(H14), C18(H18), C11(H11), C2(H2), C16(H16), C10(H10), C9(H9),
 C17(H17), C5(H5), C8(H8), C3(H3), C4(H4)
1.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37805
_olex2_submission_special_instructions 'No special instructions were received'