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_7717864
_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 H52 Al N2 O P'
_chemical_formula_sum            'C41 H52 Al N2 O P'
_chemical_formula_weight         646.79
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc2m2dqv
_audit_creation_date             2025-01-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2025-01-08 deposited with the CCDC.	2025-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.820(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8077(12)
_cell_length_b                   19.836(2)
_cell_length_c                   17.0505(18)
_cell_measurement_reflns_used    4597
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      23.61
_cell_measurement_theta_min      2.41
_cell_volume                     3801.9(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1019
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66184
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.430
_diffrn_reflns_theta_min         1.621
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.7442
_exptl_absorpt_correction_T_min  0.7069
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0823 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.9499.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0065(6)
_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   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0526P)^2^+2.2496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4884
_reflns_number_total             7801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03397c2.cif
_cod_data_source_block           myh-20
_cod_depositor_comments
'Adding full bibliography for 7717864--7717868.cif.'
_cod_original_cell_volume        3802.0(7)
_cod_database_code               7717864
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Al(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 Al1(H)
2.b Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C36(H36), C39(H39)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C28(H28), C32(H32), C33(H33),
  C34(H34)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_shelx_res_checksum              11489
_olex2_submission_special_instructions 'No special instructions were received'