Hydronium bis(trifluoromethanesulfonyl)amide–18-crown-6 (1/1)
Kitada, Atsushi; Funasako, Yusuke; Matsumoto, Kazuhiko; Hagiwara, Rika; Inokuchi, Makoto; Fukami, Kazuhiro; Murase, Kuniaki; IUCrData 5 (2020) x200162–; doi:10.1107/S2414314620001625

data_1557264
_publ_section_title
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 Hydronium bis(trifluoromethanesulfonyl)amide--18-crown-6 (1/1)
;
_journal_coeditor_code           IS4042
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x200162
_journal_paper_doi               10.1107/S2414314620001625
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          'H3 O +, C2 F6 N O4 S2 -, C12 H24 O6'
_chemical_formula_moiety         'H3 O +, C2 F6 N O4 S2 -, C12 H24 O6'
_chemical_formula_sum            'C14 H27 F6 N O11 S2'
_chemical_formula_weight         563.48
_chemical_name_systematic
;
Hydronium bis(trifluoromethanesulfonyl)amide--18-crown-6 (1/1)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 108.086(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8341(4)
_cell_length_b                   24.3932(9)
_cell_length_c                   11.6111(5)
_cell_measurement_reflns_used    22988
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      3.05
_cell_volume                     2378.47(17)
_computing_cell_refinement
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_collection
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_reduction
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID-II'
_diffrn_measurement_method       'imaging plate'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20448
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>ABSCOR</i>; Higashi, 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.535
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.45(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9354
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+5.3126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1620
_reflns_number_gt                8989
_reflns_number_total             9354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is4042sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1557264
_cod_database_fobs_code          1557264
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.938
_shelx_hkl_checksum              66850
_shelx_res_checksum              15326