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_1549756
_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         'C16 Al F36 O4, C12 H8 Ag F4'
_chemical_formula_sum            'C28 H8 Ag Al F40 O4'
_chemical_formula_weight         1303.19
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.200(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1565(5)
_cell_length_b                   18.4564(6)
_cell_length_c                   14.6510(5)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.322
_cell_measurement_theta_min      2.267
_cell_volume                     3827.1(2)
_computing_cell_refinement       'SAINT V8.34A'
_computing_data_collection       'APEX2 V2014.11-0'
_computing_data_reduction        'SAINT V8.34A'
_computing_publication_material  ShelXle-786
_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 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9266
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'INCOATEC Mo Microsourc e'
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  0.746333
_exptl_absorpt_correction_T_min  0.683262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_description       bloc
_exptl_crystal_F_000             2512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1,2-Difluorobenzene'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         9266
_refine_ls_number_restraints     3079
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0603P)^2^+2.9235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6941
_reflns_number_total             9266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc02591f2.cif
_cod_data_source_block           twin5_a
_cod_depositor_comments
'Adding full bibliography for 1549751--1549760.cif.'
_cod_database_code               1549756
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.962
_shelx_res_checksum              30245