Molecular structures of 3-[(2,2,3,3-tetrafluoropropoxy)methyl]- and 3-[(2,2,3,3,3-pentafluoropropoxy)methyl]pyridinium saccharinates
Lu, Norman; Chiang, Hsing-Fang; Wei, Rong-Jyun; Wen, Yuh-Sheng; Liu, Ling-Kang; Acta Crystallographica Section C 73 (2017) –; doi:10.1107/S2053229617009512

data_2020793
_publ_section_title
;
 Molecular structures of 3-[(2,2,3,3-tetrafluoropropoxy)methyl]- and
 3-[(2,2,3,3,3-pentafluoropropoxy)methyl]pyridinium saccharinates
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229617009512
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C9 H9 F5 N O +, C7 H4 N O3 S -'
_chemical_formula_moiety         'C9 H9 F5 N O +, C7 H4 N O3 S -'
_chemical_formula_sum            'C16 H13 F5 N2 O4 S'
_chemical_formula_weight         424.34
_chemical_name_common
;
3-[(2,2,3,3,3-Pentafluoropropoxy)methyl]pyridinium saccharinate
;
_chemical_name_systematic
;
3-[(2,2,3,3,3-Pentafluoropropoxy)methyl]pyridinium
1,1-dioxo-1\l^6^,2-benzothiazol-3-olate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.6747(6)
_cell_length_b                   21.6747(6)
_cell_length_c                   7.2850(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.51
_cell_measurement_theta_min      2.66
_cell_volume                     3422.44(19)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
shelXle (H\"ubschle <i>et al.</i>,  2011) and
ORTEP-3 (Farrugia, 2012)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            42157
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.076
_diffrn_reflns_theta_min         1.329
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_T_max  0.9705
_exptl_absorpt_correction_T_min  0.8931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.249
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1659 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0307P)^2^+2.0967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0633
_reflns_number_gt                3671
_reflns_number_total             3784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3113sup1.cif
_cod_data_source_block           i16220
_cod_original_cell_volume        3422.4(2)
_cod_database_code               2020793
_cod_database_fobs_code          2020793
_shelx_hkl_checksum              92885
_shelx_res_checksum              10872
_shelxl_version_number           .2013