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_7131062
_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         'C26 H21 Al F10 N4'
_chemical_formula_sum            'C26 H21 Al F10 N4'
_chemical_formula_weight         606.45
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 113.369(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6102(5)
_cell_length_b                   25.9241(10)
_cell_length_c                   11.8202(5)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.45
_cell_volume                     3265.9(2)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            73655
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.283
_diffrn_reflns_theta_min         2.035
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0718 before and 0.0566 after correction.
The Ratio of minimum to maximum transmission is 0.8915.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         8091
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0945P)^2^+0.4971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4448
_reflns_number_total             8091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06075b2.cif
_cod_data_source_block           final_a_sq
_cod_depositor_comments
'Adding full bibliography for 7131059--7131063.cif.'
_cod_database_code               7131062
_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, All Al(H) groups
2.a Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C20(H20), C21(H21), C23(H23), C24(H24)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13369
_shelx_hkl_checksum              71179
_shelx_fab_checksum              55244
_olex2_submission_special_instructions 'No special instructions were received'