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_7717865
_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         'C35 H55 Al N2 O2'
_chemical_formula_sum            'C35 H55 Al N2 O2'
_chemical_formula_weight         562.79
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2m2dty
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6913(4)
_cell_length_b                   17.2251(6)
_cell_length_c                   20.4705(7)
_cell_measurement_reflns_used    7818
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      74.496
_cell_measurement_theta_min      5.027
_cell_volume                     3417.2(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.1516
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27994
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.640
_diffrn_reflns_theta_min         3.353
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0769 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.9013.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2100 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.49(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         6910
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0680P)^2^+0.0910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.979
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                5733
_reflns_number_total             6910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03397c2.cif
_cod_data_source_block           cu_myh19_4_0m_a
_cod_depositor_comments
'Adding full bibliography for 7717864--7717868.cif.'
_cod_database_code               7717865
_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
 O4-C19A = O4-C19
 1.43 with sigma of 0.005
 C20A-C19A = C20-C19 = C21-C19 = C21A-C19A
 1.54 with sigma of 0.002
 C20A-C21A = C21-C20
 2.52 with sigma of 0.002
3. Others
 Fixed Sof: C19(0.5) H19(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C20(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
 C19A(0.5) H19A(0.5) C21A(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
4.a Ternary CH refined with riding coordinates:
 C34(H34), C6(H6), C9(H9), C16(H16), C30(H30), C19(H19), C19A(H19A)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C13(H13), C14(H14), C26(H26), C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F),
 C21A(H21D,H21E,H21F)
;
_shelx_res_checksum              78071
_olex2_submission_special_instructions 'No special instructions were received'