Ammonium 4,4-difluoro-1,3,2-dithiazetin-2-ide 1,1,3,3-tetraoxide
Finze, Maik; Reiss, Guido J.; Acta Crystallographica Section E 68 (2012) o1992–o1993; doi:10.1107/S1600536812024221

data_2235565
_publ_section_title
;
 Ammonium 4,4-difluoro-1,3,2-dithiazetin-2-ide 1,1,3,3-tetraoxide
;
_journal_coeditor_code           PK2414
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1992
_journal_page_last               o1993
_journal_paper_doi               10.1107/S1600536812024221
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'N H4 +, C F2 N O4 S2 -'
_chemical_formula_moiety         'H4 N +, C F2 N O4 S2 -'
_chemical_formula_sum            'C H4 F2 N2 O4 S2'
_chemical_formula_weight         210.18
_chemical_name_systematic
;
Ammonium 4,4-difluoro-1,3,2-dithiazetin-2-ide 1,1,3,3-tetraoxide
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.28642(13)
_cell_length_b                   10.98496(14)
_cell_length_c                   10.58826(12)
_cell_measurement_reflns_used    21999
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      33.59
_cell_measurement_theta_min      3.22
_cell_volume                     1312.74(3)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2011)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25817
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.232
_refine_ls_abs_structure_details 'Flack (1983), 1816 Friedel pairs'
_refine_ls_abs_structure_Flack   0.27(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3823
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.027P)^2^+0.6P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0485
_reflns_number_gt                3778
_reflns_number_total             3823
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2414.cif
_cod_data_source_block           I
_cod_database_code               2235565
_cod_database_fobs_code          2235565