The divergent reactivity of β-diketiminato aluminium hydrides with organophosphoryl compounds.
Ding, Yi; Ma, Yinghua; Tang, Yongheng; Fu, Yang; Wan, Jiayi; Xu, Zhiyuan; He, Yifei; Shi, Zhenhai; Nazish, Mohd; Wu, Peng; Roesky, Herbert W.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3827–3832; doi:10.1039/d4dt03397c

data_7717866
_publ_section_title
;
 The divergent reactivity of &#x3b2;-diketiminato aluminium hydrides with
 organophosphoryl compounds.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3827
_journal_page_last               3832
_journal_paper_doi               10.1039/d4dt03397c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C41 H51 Al N2 O2'
_chemical_formula_sum            'C41 H51 Al N2 O2'
_chemical_formula_weight         630.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2m2w1n
_audit_creation_date             2025-01-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2025-01-09 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5775(7)
_cell_length_b                   24.3473(7)
_cell_length_c                   16.4561(5)
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      70.815
_cell_measurement_theta_min      3.834
_cell_volume                     8645.3(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1383
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57909
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.805
_diffrn_reflns_theta_min         3.835
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0758 after correction.
The Ratio of minimum to maximum transmission is 0.8984.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.00023(3)
_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   0.677
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4529
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.679
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.1148
_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^)+(0.0200P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2459
_refine_ls_wR_factor_ref         0.2631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3235
_reflns_number_total             4529
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03397c2.cif
_cod_data_source_block           cu_myh16_6_0ma_a_sq
_cod_depositor_comments
'Adding full bibliography for 7717864--7717868.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7717866
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C27 = C9-C8 = C26-C25 = C19-C18 = C23-C18 = C23-C22 = C22-C21 = C21-C20 =
 C20-C19 = C25_$1-C27
 1.4 with sigma of 0.01
 C26-C10 = C8-C10
 1.4 with sigma of 0.002
3. Rigid bond restraints
 C10, C8, C26, C9, C27, C25
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C10 \\sim C8 \\sim C26 \\sim C27 \\sim C25 \\sim C9: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C8(0.5) H8(0.5) C9(0.5) H9(0.5) C25(0.5) H25(0.5) C26(0.5)
 H26(0.5) C27(0.5) H27(0.5)
6.a Ternary CH refined with riding coordinates:
 C24(H24), C6(H6)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C8(H8), C9(H9), C25(H25), C26(H26), C27(H27)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              67749
_shelx_fab_checksum              90165
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'