Theoretical and experimental studies on stability, bonding and isolation of elusive bis-(dichloro-aluminium) oxides supported by donor-base ligands
Francis, Maria; Shinde, Kishor; Roy, Sudipta; RSC Advances 15 (2025) 9208–9215; doi:10.1039/D5RA00211G

data_7250182
_publ_section_title
;
 Theoretical and experimental studies on stability, bonding and isolation
 of elusive bis-(dichloro-aluminium) oxides supported by donor-base
 ligands
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              9208
_journal_page_last               9215
_journal_paper_doi               10.1039/D5RA00211G
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C40 H62 Al2 Cl4 N2 O, C7 H7'
_chemical_formula_sum            'C47 H69 Al2 Cl4 N2 O'
_chemical_formula_weight         873.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-07-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-29 deposited with the CCDC.	2025-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                86.304(3)
_cell_angle_beta                 87.913(3)
_cell_angle_gamma                80.022(3)
_cell_formula_units_Z            1
_cell_length_a                   9.0911(7)
_cell_length_b                   10.3317(7)
_cell_length_c                   13.0377(10)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.47
_cell_volume                     1203.16(15)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            35771
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.275
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1209 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.8854.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             467
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0344P)^2^+0.7792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3559
_reflns_number_total             4251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ra00211g2.cif
_cod_data_source_block           mo_caacal_0m_a
_cod_database_code               7250182
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C23(H23), C24(H24)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              89871
_olex2_submission_special_instructions 'No special instructions were received'