Crystal structure elucidation of a geminal and vicinal bis(trifluoromethanesulfonate) ester.
Pickl, Thomas; Zuber, Julian; Stephan, Johannes; Pöthig, Alexander; Acta crystallographica. Section C, Structural chemistry 80 (2024) 278–283; doi:10.1107/S2053229624005230

data_2312522
_publ_section_title
;
 Crystal structure elucidation of a geminal and vicinal
 bis(trifluoromethanesulfonate) ester.
;
_journal_coeditor_code           OJ3019
_journal_issue                   'Pt 7'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              278
_journal_page_last               283
_journal_paper_doi               10.1107/S2053229624005230
_journal_volume                  80
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_iupac          'C3 H2 F6 O6 S2'
_chemical_formula_moiety         'C3 H2 F6 O6 S2'
_chemical_formula_sum            'C3 H2 F6 O6 S2'
_chemical_formula_weight         312.17
_chemical_melting_point          289
_chemical_name_common            'Methylene bis(triflate)'
_chemical_name_systematic
;
Methanediyl bis(trifluoromethanesulfonate)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 102.406(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9822(12)
_cell_length_b                   4.9413(6)
_cell_length_c                   10.9400(14)
_cell_measurement_reflns_used    5142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.242
_cell_measurement_theta_min      2.325
_cell_volume                     474.22(11)
_computing_cell_refinement
;
SAINT (Bruker, 2019)
;
_computing_data_collection
;
APEX4 (Bruker, 2022)
;
_computing_data_reduction
;
SAINT (Bruker, 2019)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
PLATON (Spek, 2020), enCIFer (Allen <i>et al.</i>,  2004) and
<i>FinalCif</i> (Kratzert, 2023)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b) and <i>ShelXle</i> (H\"ubschle <i>et al.</i>,
2011)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'three-angle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2295
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_min         2.322
_diffrn_source                   'TXS rotating anode'
_diffrn_source_current           50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.745686
_exptl_absorpt_correction_T_min  0.54003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(TWINABS; Bruker, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_description       plate
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.470
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 959 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.12(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2295
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0318P)^2^+0.3843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                2254
_reflns_number_total             2295
_reflns_threshold_expression     'I > 2\s(I)'
_twin_individual_id              2
_twin_individual_twin_matrix_11  0.00348
_twin_individual_twin_matrix_12  -0.0005
_twin_individual_twin_matrix_13  -1.00013
_twin_individual_twin_matrix_21  -1.0
_twin_individual_twin_matrix_22  0.00071
_twin_individual_twin_matrix_23  -0.00087
_twin_individual_twin_matrix_31  0.00242
_twin_individual_twin_matrix_32  1.00013
_twin_individual_twin_matrix_33  0.52089
_cod_data_source_file            oj3019.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2312521--2312522.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2312522
_shelx_estimated_absorpt_t_min   0.798
_shelx_estimated_absorpt_t_max   0.959
_shelx_hkl_checksum              83096
_shelx_res_checksum              37891