The Perfluoroadamantoxy Aluminate as an Ideal Weakly Coordinating Anion? – Synthesis and first Applications.
Billion, Andreas; Schorpp, Marcel; Feser, Rebecca; Schmitt, Manuel; Eisele, Lea; Scherer, Harald; Sonoda, Takaaki; Kawa, Hajimu; Butschke, Burkhard; Krossing, Ingo; Dalton Transactions  (2023) –; doi:10.1039/D3DT00199G

data_7712584
_publ_section_title
;
 The Perfluoroadamantoxy Aluminate as an Ideal Weakly Coordinating Anion?
 -- Synthesis and first Applications.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00199G
_journal_year                    2023
_chemical_formula_moiety         'C40 Al F60 O4 1-, C4 H11 O 1+, C4 H10 O'
_chemical_formula_sum            'C48 H21 Al F60 O6'
_chemical_formula_weight         1860.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V113 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.402(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.440(4)
_cell_length_b                   14.863(4)
_cell_length_c                   22.062(5)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.093
_cell_measurement_theta_min      2.2805
_cell_volume                     5857(2)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection       'Bruker BIS V6.2.12/2019-08-12'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            119781
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.126
_diffrn_reflns_theta_min         1.658
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction:
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48
(2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_description       plate
_exptl_crystal_F_000             3640
_exptl_crystal_recrystallization_method
'Crystals were obtained from a solution in 1,2-difluorobenzene at -40 \%C.'
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1091
_refine_ls_number_reflns         12932
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+20.7009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9687
_reflns_number_total             12932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00199g2.cif
_cod_data_source_block           IKmjs_RF17_a
_cod_original_cell_volume        5857(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712584
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.976
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              28225