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_7712586
_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-, C19 H15 1+, C H2 Cl2'
_chemical_formula_sum            'C60 H17 Al Cl2 F60 O4'
_chemical_formula_weight         2039.62
_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   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                 101.54(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.724(9)
_cell_length_b                   22.259(17)
_cell_length_c                   23.784(18)
_cell_measurement_reflns_used    9044
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4815
_cell_measurement_theta_min      2.2
_cell_volume                     6600(9)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS 2018.9.0.3/05-Dec-2018 && APEX3_2018.7-2'
_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 0.995
_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  0.0410
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            240992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.540
_diffrn_reflns_theta_min         1.265
_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    0.334
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7076
_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            yellow
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_recrystallization_method
'Crystals were obtained at roomtemperature by slow diffusionof pentane into a solution ofthe compound dissolved in1,2-difluorobenzene by the aidof layering.'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.073
_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     1172
_refine_ls_number_reflns         21931
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0532P)^2^+6.6430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1270
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16820
_reflns_number_total             21931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00199g2.cif
_cod_data_source_block           IKmjs_AM31_a
_cod_original_cell_volume        6600(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7712586
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.936
_olex2_diffrn_ambient_temperature_device 'Oxford Cryostream 800'
_shelx_res_checksum              14454