Polythiazide
Gelbrich, Thomas; Haddow, Mairi F.; Griesser, Ulrich J.; Acta Crystallographica Section E 66 (2010) o1663–o1664; doi:10.1107/S1600536810022105

data_2226565
_publ_section_title
;
 Polythiazide
;
_journal_coeditor_code           KJ2150
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1663
_journal_page_last               o1664
_journal_paper_doi               10.1107/S1600536810022105
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C11 H13 Cl F3 N3 O4 S3'
_chemical_formula_moiety         'C11 H13 Cl F3 N3 O4 S3'
_chemical_formula_sum            'C11 H13 Cl F3 N3 O4 S3'
_chemical_formula_weight         439.87
_chemical_name_common            polythiazide
_chemical_name_systematic
;
6-chloro-2-methyl-3-{[(2,2,2-trifluoroethyl)sulfanyl]methyl}-3,4-dihydro-
2<i>H</i>-1,2,4-benzothiadiazine-7-sulfonamide 1,1-dioxide
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.149(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6659(7)
_cell_length_b                   9.5498(6)
_cell_length_c                   13.6720(7)
_cell_measurement_reflns_used    11202
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1718.87(17)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_molecular_graphics
'XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,  2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius Roper CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9021
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.9626
_exptl_absorpt_correction_T_min  0.9271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.410
_refine_ls_abs_structure_details 'Flack (1983), 1504 Friedel pairs'
_refine_ls_abs_structure_Flack   0.12(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3197
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+0.0090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                2768
_reflns_number_total             3197
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            kj2150.cif
_cod_data_source_block           I
_cod_original_cell_volume        1718.87(16)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2226565
_cod_database_fobs_code          2226565