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_7717868
_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         'C53 H62 Al N3 O2 P2'
_chemical_formula_sum            'C53 H62 Al N3 O2 P2'
_chemical_formula_weight         861.97
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2m2dsx
_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                 94.372(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6097(7)
_cell_length_b                   19.6492(10)
_cell_length_c                   21.1472(13)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.20
_cell_volume                     4810.1(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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50439
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.398
_diffrn_reflns_theta_min         1.759
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0645 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.9277.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 5764 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1119
_refine_ls_number_reflns         18488
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.6328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                14724
_reflns_number_total             18488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03397c2.cif
_cod_data_source_block           mo_myh21_3_0m_a
_cod_depositor_comments
'Adding full bibliography for 7717864--7717868.cif.'
_cod_database_code               7717868
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C31(H31), C38(H38), C47(H47), C50(H50), C60(H60), C69(H69), C76(H76),
 C103(H103)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C106(H106), N5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C26(H26), C34(H34), C35(H35), C36(H36),
 C43(H43), C44(H44), C45(H45), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C65(H65), C72(H72), C73(H73), C74(H74), C80(H80), C81(H81), C82(H82),
 C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90),
  C91(H91), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97), C100(H100),
 C101(H101), C102(H102), N3(H3)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C61(H61A,H61B,H61C),
 C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C98(H98A,H98B,H98C),
 C104(H10A,H10B,H10C), C105(H10D,H10E,H10F)
;
_shelx_res_checksum              55430
_olex2_submission_special_instructions 'No special instructions were received'