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_7712585
_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_absolute_configuration ad
_chemical_formula_moiety         'C40 Al F60 O4, C20 Ag3 F30 O2, 5(C6 H4 F2)'
_chemical_formula_sum            'C90 H20 Ag3 Al F100 O6'
_chemical_formula_weight         3447.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9498(7)
_cell_length_b                   18.4428(12)
_cell_length_c                   36.6960(19)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.235
_cell_measurement_theta_min      2.28
_cell_volume                     10117.7(10)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS 2018.9.0.3/05-Dec-2018 && APEX2_2014.11-0'
_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                 CCD
_diffrn_detector_area_resol_mean 8.3
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 QUAZAR'
_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  0.0293
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            91049
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.711
_diffrn_reflns_theta_min         1.110
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.6
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6959
_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    2.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             6648
_exptl_crystal_recrystallization_method
'Crystals were obtained at room temperature by slow diffusion of pentane into asolution of the compound dissolved in 1,2-difluorobenzene by the aid oflayering.'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.447(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3609
_refine_ls_number_reflns         25175
_refine_ls_number_restraints     68351
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+16.4196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                22252
_reflns_number_total             25175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00199g2.cif
_cod_data_source_block           IKmjs_AM11_a
_cod_database_code               7712585
_shelx_shelxl_version_number     2018/3
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              80348