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_7131060
_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         'C23 H9 Al F10 O, C6 H5 Cl'
_chemical_formula_sum            'C29 H14 Al Cl F10 O'
_chemical_formula_weight         630.83
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-29 deposited with the CCDC.	2022-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                110.793(2)
_cell_angle_beta                 104.745(2)
_cell_angle_gamma                107.462(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3773(5)
_cell_length_b                   11.6740(5)
_cell_length_c                   11.8396(5)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      70.104
_cell_measurement_theta_min      4.369
_cell_volume                     1282.29(11)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      150.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17723
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.132
_diffrn_reflns_theta_min         4.368
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.552
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chlorobenzene and hexane'
_refine_diff_density_max         1.183
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0768P)^2^+0.9868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4504
_reflns_number_total             4860
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06075b2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7131059--7131063.cif.'
_cod_original_cell_volume        1282.28(10)
_cod_database_code               7131060
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C27(H27), C25(H25), C4(H4), C26(H26), C29(H29), C11(H11),
 C8(H8), C10(H10), C28(H28), C9(H9)
;
_shelx_res_checksum              12475
_shelx_hkl_checksum              18401
_olex2_submission_special_instructions 'No special instructions were received'