Facile and systematic access to the least-coordinating WCA [(R<sup>F</sup>O)<sub>3</sub>Al-F-Al(OR<sup>F</sup>)<sub>3</sub>]<sup>-</sup> and its more Lewis-basic brother [F-Al(OR<sup>F</sup>)<sub>3</sub>]<sup>-</sup> (R<sup>F</sup> = C(CF<sub>3</sub>)<sub>3</sub>).
Martens, Arthur; Weis, Philippe; Krummer, Michael Christian; Kreuzer, Marvin; Meierhöfer, Andreas; Meier, Stefan C.; Bohnenberger, Jan; Scherer, Harald; Riddlestone, Ian; Krossing, Ingo; Chemical science 9 (2018) 7058–7068; doi:10.1039/c8sc02591f

data_1549759
_publ_section_title
;
 Facile and systematic access to the least-coordinating WCA
 [(R<sup>F</sup>O)<sub>3</sub>Al-F-Al(OR<sup>F</sup>)<sub>3</sub>]<sup>-</sup>
 and its more Lewis-basic brother
 [F-Al(OR<sup>F</sup>)<sub>3</sub>]<sup>-</sup> (R<sup>F</sup> =
 C(CF<sub>3</sub>)<sub>3</sub>).
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              7058
_journal_page_last               7068
_journal_paper_doi               10.1039/c8sc02591f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C21 H18 Al F28 Li O12'
_chemical_formula_sum            'C21 H18 Al F28 Li O12'
_chemical_formula_weight         1028.27
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-28 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.381(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.9221(16)
_cell_length_b                   10.7468(5)
_cell_length_c                   19.3985(9)
_cell_measurement_reflns_used    9021
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      48.987
_cell_measurement_theta_min      4.644
_cell_volume                     7314.6(6)
_computing_cell_refinement       'SAINT V8.34A'
_computing_data_collection       'APEX3 v2016.5-0'
_computing_data_reduction        'SAINT V8.34A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5, Sheldrick, 2014'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            256191
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         1.161
_diffrn_source                   'INCOATEC Mo Microsouce'
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_description       needle
_exptl_crystal_F_000             4064
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-Difluorobenzen2/CH2Cl2/Cl3CCN'
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1458
_refine_ls_number_reflns         13451
_refine_ls_number_restraints     11779
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0404P)^2^+11.4394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10618
_reflns_number_total             13451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02591f2.cif
_cod_data_source_block           p21c_a
_cod_depositor_comments
'Adding full bibliography for 1549751--1549760.cif.'
_cod_database_code               1549759
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.965
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              18734