Structure and reactivity studies of the aluminum analogue of Piers' borane [HAl(C<sub>6</sub>F<sub>5</sub>)<sub>2</sub>]<sub>3</sub>.
Tan, Jingjie; Hu, Chaopeng; Yang, Xin; Ju, Shaoying; Cao, Levy L.; Wu, Yile; Liu, Liu Leo; Stephan, Douglas W.; Chemical communications (Cambridge, England) 59 (2023) 282–285; doi:10.1039/d2cc06075b

data_7131061
_publ_section_title
;
 Structure and reactivity studies of the aluminum analogue of Piers'
 borane [HAl(C<sub>6</sub>F<sub>5</sub>)<sub>2</sub>]<sub>3</sub>.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              282
_journal_page_last               285
_journal_paper_doi               10.1039/d2cc06075b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C40 H8 Al2 Br2 F20'
_chemical_formula_sum            'C40 H8 Al2 Br2 F20'
_chemical_formula_weight         1082.24
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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             2022-04-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-07 deposited with the CCDC.	2022-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                86.250(2)
_cell_angle_beta                 63.214(2)
_cell_angle_gamma                61.222(2)
_cell_formula_units_Z            1
_cell_length_a                   10.8687(4)
_cell_length_b                   11.0798(5)
_cell_length_c                   11.7308(5)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      70.13
_cell_measurement_theta_min      4.30
_cell_volume                     1084.39(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            38344
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.315
_diffrn_reflns_theta_min         4.303
_exptl_absorpt_coefficient_mu    3.836
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene and hexane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4129
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0453P)^2^+0.6851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3946
_reflns_number_total             4129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06075b2.cif
_cod_data_source_block           11_sq
_cod_depositor_comments
'Adding full bibliography for 7131059--7131063.cif.'
_cod_original_cell_volume        1084.39(8)
_cod_database_code               7131061
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Restrained distances
 Br01-C6 \\sim Br1-C6
 with sigma of 0.02
2. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Br01)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10875
_shelx_hkl_checksum              10610
_shelx_fab_checksum              90384
_olex2_submission_special_instructions 'No special instructions were received'