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_1552376
_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_formula_moiety         'C16 Al1 Cl3 F36 O4 Se1'
_chemical_formula_sum            'C16 Al Cl3 F36 O4 Se'
_chemical_formula_weight         1152.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-20 deposited with the CCDC.    2019-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.9650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   16.5135(7)
_cell_length_b                   31.9553(16)
_cell_length_c                   19.1323(9)
_cell_measurement_reflns_used    9358
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.424
_cell_measurement_theta_min      2.213
_cell_volume                     9706.6(8)
_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 0.998
_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_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            225399
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.084
_diffrn_reflns_theta_min         0.637
_diffrn_source                   'INCOATEC Mo Microsource'
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7016
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             6600
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.865
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 13075 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0065(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3461
_refine_ls_number_reflns         40927
_refine_ls_number_restraints     95750
_refine_ls_restrained_S_all      0.844
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0728P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                32319
_reflns_number_total             40927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03915e2.cif
_cod_data_source_block           Pn_a
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 Al6 Cl18 F216 O24 Se5.99'
_cod_original_formula_weight         6914.23
_cod_original_formula_units_Z            2
_cod_database_code               1552376
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.921
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              7743