The Lewis superacidic aluminium cation: [(NHC)Al(C<sub>6</sub>F<sub>5</sub>)<sub>2</sub>]<sup/>.
Ju, Shaoying; Zhang, Chi; Tang, Beili; Liu, Liu Leo; Stephan, Douglas W.; Wu, Yile; Chemical communications (Cambridge, England) 60 (2024) 698–701; doi:10.1039/d3cc05440c

data_7132430
_publ_section_title
;
 The Lewis superacidic aluminium cation:
 [(NHC)Al(C<sub>6</sub>F<sub>5</sub>)<sub>2</sub>]<sup/>.
;
_journal_issue                   6
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              698
_journal_page_last               701
_journal_paper_doi               10.1039/d3cc05440c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'B C24 F20, C46 H44 Al F10 N2, C7 H8'
_chemical_formula_sum            'C77 H52 Al B F30 N2'
_chemical_formula_weight         1612.99
_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             2023-09-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-12 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                75.193(2)
_cell_angle_beta                 78.870(2)
_cell_angle_gamma                70.815(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8701(5)
_cell_length_b                   14.0245(6)
_cell_length_c                   21.8859(9)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      67.97
_cell_measurement_theta_min      3.62
_cell_volume                     3581.2(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0636
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            148386
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         2.103
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.8797.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       block
_exptl_crystal_F_000             1632
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1266
_refine_ls_number_reflns         12648
_refine_ls_number_restraints     494
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0761P)^2^+5.5144P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10807
_reflns_number_total             12648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc05440c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7132428--7132432.cif.'
_cod_database_code               7132430
_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
2. Restrained distances
 C1-C5 \\sim C1A-C5A
 with sigma of 0.02
 C1-C6 \\sim C1A-C6A
 with sigma of 0.02
 C2-C3 \\sim C2A-C3A
 with sigma of 0.02
 C2-C4 \\sim C2A-C4A
 with sigma of 0.02
 C3-C5 \\sim C3A-C5A
 with sigma of 0.02
 C3-C8 \\sim C3A-C8A
 with sigma of 0.02
 C4-C6 \\sim C4A-C6A
 with sigma of 0.02
 C1-C3 \\sim C1A-C3A
 with sigma of 0.04
 C1-C4 \\sim C1A-C4A
 with sigma of 0.04
 C2-C5 \\sim C2A-C5A
 with sigma of 0.04
 C2-C6 \\sim C2A-C6A
 with sigma of 0.04
 C2-C8 \\sim C2A-C8A
 with sigma of 0.04
 C3-C4 \\sim C3A-C4A
 with sigma of 0.04
 C5-C6 \\sim C5A-C6A
 with sigma of 0.04
 C5-C8 \\sim C5A-C8A
 with sigma of 0.04
 C6A-C4A \\sim C6B-C4B
 with sigma of 0.02
 C6A-C1A \\sim C6B-C1B
 with sigma of 0.02
 C4A-C2A \\sim C4B-C2B
 with sigma of 0.02
 C2A-C3A \\sim C2B-C3B
 with sigma of 0.02
 C3A-C5A \\sim C3B-C5B
 with sigma of 0.02
 C3A-C8A \\sim C3B-C8B
 with sigma of 0.02
 C5A-C1A \\sim C5B-C1B
 with sigma of 0.02
 C6A-C2A \\sim C6B-C2B
 with sigma of 0.04
 C6A-C5A \\sim C6B-C5B
 with sigma of 0.04
 C4A-C3A \\sim C4B-C3B
 with sigma of 0.04
 C4A-C1A \\sim C4B-C1B
 with sigma of 0.04
 C2A-C5A \\sim C2B-C5B
 with sigma of 0.04
 C2A-C8A \\sim C2B-C8B
 with sigma of 0.04
 C3A-C1A \\sim C3B-C1B
 with sigma of 0.04
 C5A-C8A \\sim C5B-C8B
 with sigma of 0.04
 C024-C02E \\sim C12-C7
 with sigma of 0.02
 C026-C027 \\sim C0-C10
 with sigma of 0.02
 C026-C02L \\sim C0-C9
 with sigma of 0.02
 C02E-C02L \\sim C7-C9
 with sigma of 0.02
 C02E-C02W \\sim C7-C02X
 with sigma of 0.02
 C024-C027 \\sim C12-C10
 with sigma of 0.04
 C024-C02L \\sim C12-C9
 with sigma of 0.04
 C024-C02W \\sim C12-C02X
 with sigma of 0.04
 C026-C02E \\sim C0-C7
 with sigma of 0.04
 C027-C02L \\sim C10-C9
 with sigma of 0.04
 C02L-C02W \\sim C9-C02X
 with sigma of 0.04
 F00R-C02H \\sim F00S-C15
 with sigma of 0.02
 F00U-C02P \\sim F00V-C13
 with sigma of 0.02
 F01T-C02T \\sim F01U-C17
 with sigma of 0.02
 C022-C02H \\sim C14-C15
 with sigma of 0.02
 C022-C02P \\sim C14-C13
 with sigma of 0.02
 C022-Al1 \\sim C14-Al1
 with sigma of 0.02
 C02H-C02T \\sim C15-C17
 with sigma of 0.02
 F02J-C02U \\sim F02K-C16
 with sigma of 0.02
 F02O-C02V \\sim F02P-C18
 with sigma of 0.02
 C02P-C02V \\sim C13-C18
 with sigma of 0.02
 C02T-C02U \\sim C17-C16
 with sigma of 0.02
 C02U-C02V \\sim C16-C18
 with sigma of 0.02
 F00R-C022 \\sim F00S-C14
 with sigma of 0.04
 F00R-C02T \\sim F00S-C17
 with sigma of 0.04
 F00U-C022 \\sim F00V-C14
 with sigma of 0.04
 F00U-C02V \\sim F00V-C18
 with sigma of 0.04
 F01T-C02H \\sim F01U-C15
 with sigma of 0.04
 F01T-C02U \\sim F01U-C16
 with sigma of 0.04
 C022-C02T \\sim C14-C17
 with sigma of 0.04
 C022-C02V \\sim C14-C18
 with sigma of 0.04
 C02H-C02P \\sim C15-C13
 with sigma of 0.04
 C02H-C02U \\sim C15-C16
 with sigma of 0.04
 C02H-Al1 \\sim C15-Al1
 with sigma of 0.04
 F02J-C02T \\sim F02K-C17
 with sigma of 0.04
 F02J-C02V \\sim F02K-C18
 with sigma of 0.04
 F02O-C02P \\sim F02P-C13
 with sigma of 0.04
 F02O-C02U \\sim F02P-C16
 with sigma of 0.04
 C02P-C02U \\sim C13-C16
 with sigma of 0.04
 C02P-Al1 \\sim C13-Al1
 with sigma of 0.04
 C02T-C02V \\sim C17-C18
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C4A \\sim C3A \\sim C5A \\sim C2A \\sim C8A \\sim C1A \\sim C6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C4B \\sim C8B \\sim C3B \\sim C2B \\sim C5B \\sim C1B \\sim C6B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C6 \\sim C1 \\sim C5 \\sim C3 \\sim C4 \\sim C2 \\sim C8: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
C027 \\sim C026 \\sim C02L \\sim C021 \\sim C02E \\sim C024 \\sim C02W: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C7 \\sim C02X \\sim C9 \\sim C12 \\sim C0 \\sim C11 \\sim C10: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Al1 \\sim F00R \\sim C02H \\sim C02T \\sim C022 \\sim C02U \\sim F01T \\sim
C02P \\sim F02J \\sim C02V \\sim F00U \\sim F02O: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C14 \\sim F00V \\sim C13 \\sim C18 \\sim C15 \\sim C16 \\sim F02P \\sim F00S
\\sim C17 \\sim F02K \\sim F01U: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
C023 \\sim C02M \\sim F00P \\sim F01C \\sim C02S \\sim C02R \\sim C02N \\sim
F00Q \\sim F01B \\sim C028 \\sim F00F: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Others
 Sof(F00V)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(F00S)=Sof(F01U)=Sof(C16)=Sof(C17)=
 Sof(F02K)=Sof(C18)=Sof(F02P)=1-FVAR(1)
 Sof(F00R)=Sof(F00U)=Sof(F01T)=Sof(C022)=Sof(C02H)=Sof(F02J)=Sof(F02O)=
 Sof(C02P)=Sof(C02T)=Sof(C02U)=Sof(C02V)=FVAR(1)
 Fixed Sof: C026(0.5) H026(0.5) C027(0.5) H027(0.5) C021(0.5) H021(0.5)
 C024(0.5) H024(0.5) C02E(0.5) C02L(0.5) H02L(0.5) C02W(0.5) H02Z(0.5) HA(0.5)
 HB(0.5) C1(0.35) H1(0.35) C5(0.35) H5(0.35) C3(0.35) C2(0.35) H2(0.35)
 C4(0.35) H4(0.35) C6(0.35) H6(0.35) C8(0.35) H8A(0.35) H8B(0.35) H8C(0.35)
 C3A(0.25) C5A(0.25) H5A(0.25) C1A(0.25) H1A(0.25) C6A(0.25) H6A(0.25)
 C4A(0.25) H4A(0.25) C2A(0.25) H2A(0.25) C8A(0.25) H8AA(0.25) H8AB(0.25)
 H8AC(0.25) C8B(0.4) H8BA(0.4) H8BB(0.4) H8BC(0.4) C6B(0.4) H6B(0.4) C4B(0.4)
 H4B(0.4) C1B(0.4) H1B(0.4) C2B(0.4) H2B(0.4) C5B(0.4) H5B(0.4) C3B(0.4)
 C02X(0.5) H02(0.5) HC(0.5) HD(0.5) C7(0.5) C9(0.5) H9(0.5) C0(0.5) H0(0.5)
 C10(0.5) H10(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5)
5.a Ternary CH refined with riding coordinates:
 C01K(H01K), C01U(H01U), C01V(H01V), C01Y(H01Y)
5.b Aromatic/amide H refined with riding coordinates:
 C011(H011), C014(H014), C01L(H01L), C01Q(H01Q), C01W(H01W), C01X(H01X),
 C026(H026), C027(H027), C021(H021), C024(H024), C02L(H02L), C029(H029),
 C02F(H02N), C1(H1), C5(H5), C2(H2), C4(H4), C6(H6), C5A(H5A), C1A(H1A),
 C6A(H6A), C4A(H4A), C2A(H2A), C6B(H6B), C4B(H4B), C1B(H1B), C2B(H2B), C5B(H5B),
  C9(H9), C0(H0), C10(H10), C12(H12), C11(H11)
5.c Fitted hexagon refined as free rotating group:
 C026(C027,C021,C024,C02E,C02L), C1(C5,C3,C2,C4,C6), C3A(C5A,C1A,C6A,C4A,C2A)
5.d Idealised Me refined as rotating group:
 C025(H02A,H02B,H02C), C02A(H02D,H02E,H02F), C02B(H02G,H02H,H02I), C02D(H02J,
 H02K,H02M), C02G(H02O,H02P,H02Q), C02I(H02R,H02S,H02T), C02K(H02U,H02V,H02W),
 C02Q(H02X,H02Y,H), C02W(H02Z,HA,HB), C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC),
 C8B(H8BA,H8BB,H8BC), C02X(H02,HC,HD)
;
_shelx_res_checksum              42245
_shelx_hkl_checksum              69547
_olex2_submission_special_instructions 'No special instructions were received'