#------------------------------------------------------------------------------
#$Date: 2023-05-05 03:43:18 +0300 (Fri, 05 May 2023) $
#$Revision: 283142 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/10/7131061.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7131061
loop_
_publ_author_name
'Tan, Jingjie'
'Hu, Chaopeng'
'Yang, Xin'
'Ju, Shaoying'
'Cao, Levy L.'
'Wu, Yile'
'Liu, Liu Leo'
'Stephan, Douglas W.'
_publ_section_title
;
 Structure and reactivity studies of the aluminum analogue of Piers'
 borane [HAl(C₆F₅)₂]₃.
;
_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       'φ and ω 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/[σ²(Fo²)+(0.0453P)²+0.6851P] where P=(Fo²+2Fc²)/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 > 2σ(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
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br01 Br 0.4075(2) -0.3314(2) 0.58694(17) 0.0268(5) Uani 0.341(9) 1 d D . P A 1
Al1 Al 0.93972(7) 0.14237(6) 0.47347(5) 0.02602(13) Uani 1 1 d . . . . .
F5 F 0.97429(14) 0.37497(12) 0.55060(12) 0.0361(3) Uani 1 1 d . . . . .
F1 F 0.56994(14) 0.25750(13) 0.70114(11) 0.0356(3) Uani 1 1 d . . . . .
F10 F 1.22741(16) -0.06350(13) 0.21355(11) 0.0410(3) Uani 1 1 d . . . . .
F4 F 0.77747(16) 0.60130(13) 0.74616(14) 0.0445(3) Uani 1 1 d . . . . .
F2 F 0.37830(14) 0.48006(14) 0.89600(12) 0.0444(3) Uani 1 1 d . . . . .
F6 F 0.85571(16) 0.42244(13) 0.35669(12) 0.0425(3) Uani 1 1 d . . . . .
F3 F 0.48005(16) 0.65289(13) 0.92105(13) 0.0463(3) Uani 1 1 d . . . . .
F9 F 1.37403(18) -0.01942(17) -0.02589(12) 0.0567(4) Uani 1 1 d . . . . .
F7 F 1.0008(3) 0.46537(18) 0.11879(17) 0.0734(5) Uani 1 1 d . . . . .
F8 F 1.2606(3) 0.2444(2) -0.07600(15) 0.0832(6) Uani 1 1 d . . . . .
C1 C 0.8748(2) -0.00200(18) 0.48259(15) 0.0213(3) Uani 1 1 d . . . . .
C10 C 0.6282(2) 0.3383(2) 0.70960(19) 0.0297(4) Uani 1 1 d . . . . .
C9 C 0.7817(2) 0.30614(19) 0.61853(18) 0.0272(4) Uani 1 1 d . . . . .
C15 C 1.0379(2) 0.1777(2) 0.29626(18) 0.0285(4) Uani 1 1 d . . . . .
C14 C 0.8256(2) 0.3991(2) 0.63522(19) 0.0298(4) Uani 1 1 d . . . . .
C20 C 1.1696(2) 0.0698(2) 0.19368(19) 0.0321(4) Uani 1 1 d . . . . .
C11 C 0.5264(2) 0.4529(2) 0.81069(19) 0.0329(4) Uani 1 1 d . . . . .
C3 C 0.6935(2) -0.11069(19) 0.52428(19) 0.0288(4) Uani 1 1 d . . . . .
C2 C 0.7908(2) -0.05035(19) 0.50048(17) 0.0283(4) Uani 1 1 d . . . . .
C13 C 0.7282(3) 0.5151(2) 0.7343(2) 0.0332(4) Uani 1 1 d . . . . .
C4 C 0.5845(3) -0.0994(2) 0.6512(2) 0.0343(4) Uani 1 1 d . . . . .
H4 H 0.572418 -0.049158 0.721717 0.041 Uiso 1 1 calc R U . . .
C12 C 0.5771(3) 0.5410(2) 0.8235(2) 0.0345(4) Uani 1 1 d . . . . .
C16 C 0.9848(3) 0.3098(2) 0.2648(2) 0.0341(4) Uani 1 1 d . . . . .
C5 C 0.4937(3) -0.1616(2) 0.6746(2) 0.0401(5) Uani 1 1 d . . . . .
H5 H 0.418620 -0.154595 0.760968 0.048 Uiso 1 1 calc R U . . .
C8 C 0.7096(3) -0.1837(2) 0.4203(2) 0.0366(5) Uani 1 1 d . . . . .
H8 H 0.783372 -0.190524 0.333444 0.044 Uiso 1 1 calc R U . . .
C19 C 1.2464(3) 0.0892(3) 0.0694(2) 0.0419(5) Uani 1 1 d . . . . .
C7 C 0.6189(3) -0.2454(2) 0.4437(2) 0.0396(5) Uani 1 1 d . . . . .
H7 H 0.628883 -0.294605 0.373776 0.047 Uiso 1 1 calc R U . . .
C6 C 0.5138(3) -0.2343(2) 0.5701(3) 0.0398(5) Uani 1 1 d D . . . .
C17 C 1.0571(3) 0.3345(3) 0.1419(2) 0.0474(6) Uani 1 1 d . . . . .
C18 C 1.1883(4) 0.2236(3) 0.0443(2) 0.0524(6) Uani 1 1 d . . . . .
Br1 Br 0.3815(4) -0.3171(3) 0.6139(4) 0.0649(4) Uani 0.659(9) 1 d D . P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Al1 Al1 43.57(5) 2_756 2_756 ?
C1 Al1 Al1 46.90(5) . 2_756 ?
C1 Al1 C1 90.46(7) . 2_756 ?
C9 Al1 Al1 120.30(6) . 2_756 ?
C9 Al1 C1 108.30(7) . 2_756 ?
C9 Al1 C1 113.54(8) . . ?
C9 Al1 C15 117.88(8) . . ?
C15 Al1 Al1 121.09(7) . 2_756 ?
C15 Al1 C1 108.84(7) . 2_756 ?
C15 Al1 C1 114.03(8) . . ?
Al1 C1 Al1 89.54(7) . 2_756 ?
C2 C1 Al1 159.48(15) . . ?
C2 C1 Al1 108.05(14) . 2_756 ?
F1 C10 C9 120.31(17) . . ?
F1 C10 C11 116.43(17) . . ?
C11 C10 C9 123.25(19) . . ?
C10 C9 Al1 126.74(15) . . ?
C14 C9 Al1 118.40(14) . . ?
C14 C9 C10 114.86(17) . . ?
C20 C15 Al1 121.51(14) . . ?
C20 C15 C16 114.74(17) . . ?
C16 C15 Al1 123.74(15) . . ?
F5 C14 C9 118.69(17) . . ?
F5 C14 C13 117.23(18) . . ?
C13 C14 C9 124.07(18) . . ?
F10 C20 C15 119.23(17) . . ?
F10 C20 C19 116.87(19) . . ?
C19 C20 C15 123.9(2) . . ?
F2 C11 C10 120.96(19) . . ?
F2 C11 C12 119.62(18) . . ?
C12 C11 C10 119.42(18) . . ?
C4 C3 C2 119.69(18) . . ?
C4 C3 C8 119.92(19) . . ?
C8 C3 C2 120.38(18) . . ?
C1 C2 C3 178.02(19) . . ?
F4 C13 C14 121.50(19) . . ?
F4 C13 C12 119.92(18) . . ?
C14 C13 C12 118.58(19) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4 120.2 . . ?
F3 C12 C11 120.37(19) . . ?
F3 C12 C13 119.8(2) . . ?
C11 C12 C13 119.81(18) . . ?
F6 C16 C15 119.86(17) . . ?
F6 C16 C17 116.64(19) . . ?
C17 C16 C15 123.5(2) . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.0(2) . . ?
C6 C5 H5 120.5 . . ?
C3 C8 H8 119.8 . . ?
C7 C8 C3 120.3(2) . . ?
C7 C8 H8 119.8 . . ?
F9 C19 C20 121.2(2) . . ?
F9 C19 C18 120.22(19) . . ?
C20 C19 C18 118.6(2) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 C8 118.6(2) . . ?
C6 C7 H7 120.7 . . ?
C5 C6 Br01 123.81(19) . . ?
C5 C6 Br1 115.5(2) . . ?
C7 C6 Br01 113.62(18) . . ?
C7 C6 C5 122.5(2) . . ?
C7 C6 Br1 122.0(2) . . ?
F7 C17 C16 120.4(2) . . ?
F7 C17 C18 120.5(2) . . ?
C18 C17 C16 119.2(2) . . ?
F8 C18 C19 119.5(2) . . ?
F8 C18 C17 120.4(2) . . ?
C17 C18 C19 120.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br01 C6 1.869(3) . ?
Al1 Al1 2.9249(11) 2_756 ?
Al1 C1 2.0159(18) . ?
Al1 C1 2.1356(18) 2_756 ?
Al1 C9 1.9767(19) . ?
Al1 C15 1.9774(19) . ?
F5 C14 1.357(2) . ?
F1 C10 1.352(2) . ?
F10 C20 1.351(2) . ?
F4 C13 1.340(2) . ?
F2 C11 1.343(2) . ?
F6 C16 1.347(3) . ?
F3 C12 1.341(2) . ?
F9 C19 1.339(3) . ?
F7 C17 1.340(3) . ?
F8 C18 1.339(3) . ?
C1 C2 1.204(3) . ?
C10 C9 1.386(3) . ?
C10 C11 1.379(3) . ?
C9 C14 1.382(3) . ?
C15 C20 1.383(3) . ?
C15 C16 1.386(3) . ?
C14 C13 1.379(3) . ?
C20 C19 1.380(3) . ?
C11 C12 1.375(3) . ?
C3 C2 1.426(3) . ?
C3 C4 1.389(3) . ?
C3 C8 1.405(3) . ?
C13 C12 1.382(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(3) . ?
C16 C17 1.380(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(3) . ?
C8 H8 0.9500 . ?
C8 C7 1.376(3) . ?
C19 C18 1.381(4) . ?
C7 H7 0.9500 . ?
C7 C6 1.372(4) . ?
C6 Br1 1.927(3) . ?
C17 C18 1.371(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 C9 C14 F5 0.8(2) . . . . ?
Al1 C9 C14 C13 -178.27(16) . . . . ?
Al1 C15 C20 F10 3.4(3) . . . . ?
Al1 C15 C20 C19 -177.48(17) . . . . ?
Al1 C15 C16 F6 -2.5(3) . . . . ?
Al1 C15 C16 C17 177.78(18) . . . . ?
F5 C14 C13 F4 0.6(3) . . . . ?
F5 C14 C13 C12 -178.84(17) . . . . ?
F1 C10 C9 Al1 -3.2(3) . . . . ?
F1 C10 C9 C14 178.04(16) . . . . ?
F1 C10 C11 F2 0.7(3) . . . . ?
F1 C10 C11 C12 -178.77(17) . . . . ?
F10 C20 C19 F9 -1.2(3) . . . . ?
F10 C20 C19 C18 178.3(2) . . . . ?
F4 C13 C12 F3 0.4(3) . . . . ?
F4 C13 C12 C11 179.61(18) . . . . ?
F2 C11 C12 F3 0.6(3) . . . . ?
F2 C11 C12 C13 -178.64(18) . . . . ?
F6 C16 C17 F7 1.3(3) . . . . ?
F6 C16 C17 C18 -179.5(2) . . . . ?
F9 C19 C18 F8 0.0(4) . . . . ?
F9 C19 C18 C17 179.7(2) . . . . ?
F7 C17 C18 F8 -1.0(4) . . . . ?
F7 C17 C18 C19 179.3(2) . . . . ?
C10 C9 C14 F5 179.70(16) . . . . ?
C10 C9 C14 C13 0.6(3) . . . . ?
C10 C11 C12 F3 180.00(18) . . . . ?
C10 C11 C12 C13 0.8(3) . . . . ?
C9 C10 C11 F2 179.56(18) . . . . ?
C9 C10 C11 C12 0.1(3) . . . . ?
C9 C14 C13 F4 179.65(18) . . . . ?
C9 C14 C13 C12 0.2(3) . . . . ?
C15 C20 C19 F9 179.6(2) . . . . ?
C15 C20 C19 C18 -0.8(4) . . . . ?
C15 C16 C17 F7 -179.0(2) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C14 C13 C12 F3 179.82(18) . . . . ?
C14 C13 C12 C11 -1.0(3) . . . . ?
C20 C15 C16 F6 178.88(18) . . . . ?
C20 C15 C16 C17 -0.8(3) . . . . ?
C20 C19 C18 F8 -179.5(2) . . . . ?
C20 C19 C18 C17 0.1(4) . . . . ?
C11 C10 C9 Al1 177.97(15) . . . . ?
C11 C10 C9 C14 -0.8(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C3 C8 C7 C6 -0.3(3) . . . . ?
C2 C3 C4 C5 -178.01(19) . . . . ?
C2 C3 C8 C7 178.09(18) . . . . ?
C4 C3 C8 C7 -0.6(3) . . . . ?
C4 C5 C6 Br01 176.73(18) . . . . ?
C4 C5 C6 C7 -1.0(3) . . . . ?
C4 C5 C6 Br1 179.87(17) . . . . ?
C16 C15 C20 F10 -178.00(18) . . . . ?
C16 C15 C20 C19 1.1(3) . . . . ?
C16 C17 C18 F8 179.8(2) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C8 C3 C4 C5 0.7(3) . . . . ?
C8 C7 C6 Br01 -176.85(17) . . . . ?
C8 C7 C6 C5 1.1(3) . . . . ?
C8 C7 C6 Br1 -179.83(17) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 161.4 47.1 ?
