First Experimental Evidence for the Elusive Tetrahedral Cations [EP3]+ in the Condensed Phase
Weis, Philippe; Röhner, David C.; Prediger, Richard; Butschke, Burkhard; Scherer, Harald; Weber, Stefan; Krossing, Ingo; Chemical Science  (2019) –; doi:10.1039/C9SC03915E

data_1552374
_publ_section_title
;
 First Experimental Evidence for the Elusive Tetrahedral Cations [EP3]+ in
 the Condensed Phase
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03915E
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 Al F36 O4, Tl'
_chemical_formula_sum            'C16 Al F36 O4 Tl'
_chemical_formula_weight         1171.51
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-02-20 deposited with the CCDC.    2019-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                81.433(2)
_cell_angle_beta                 73.4860(10)
_cell_angle_gamma                63.3710(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6336(2)
_cell_length_b                   10.4764(3)
_cell_length_c                   16.8374(4)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.458
_cell_measurement_theta_min      2.440
_cell_volume                     1455.95(6)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       'APEX2 v2014.11-0'
_computing_data_reduction        'SAINT V8.37A'
_computing_publication_material  ShelXle-924
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5, Sheldrick, 2014'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.764
_diffrn_measurement_device_type  'Bruker Smart Apex2 Quazar'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.764
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            46434
_diffrn_reflns_point_group_measured_fraction_full 0.901
_diffrn_reflns_point_group_measured_fraction_max 0.610
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.256
_diffrn_reflns_theta_min         1.262
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    5.838
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.672
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 4359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1155
_refine_ls_number_reflns         12615
_refine_ls_number_restraints     12837
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0389P)^2^+3.6976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.598
_reflns_Friedel_fraction_full    0.804
_reflns_Friedel_fraction_max     0.456
_reflns_number_gt                12053
_reflns_number_total             12615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03915e2.cif
_cod_data_source_block           fin
_cod_database_code               1552374
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.420
_shelx_estimated_absorpt_t_max   0.593
_shelx_res_checksum              37676