Crystal structure of 2-(4-nitroanilino)-4,5,6,7-tetrahydro-1,2-benzisothiazolium perchlorate, [C13H14N3O2S][ClO4]
Valeria M. Zakharova; Joachim Sieler; Bärbel Schulze; Zeitschrift für Kristallographie - New Crystal Structures 224 (2009) 133–; doi:

data_8103025
_publ_section_title
;
 Crystal structure of
 2-(4-nitroanilino)-4,5,6,7-tetrahydro-1,2-benzisothiazolium
 perchlorate, [C13H14N3O2S][ClO4]
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              133
_journal_volume                  224
_journal_year                    2009
_chemical_formula_sum            'C13 H14 Cl N3 O6 S'
_chemical_formula_weight         375.78
_chemical_name_systematic
;
  2-(4-nitroanilino)-4,5,6,7-tetrahydro-1,2-benzisothiazolium perchloate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 104.600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3480(10)
_cell_length_b                   15.657(2)
_cell_length_c                   12.680(2)
_cell_measurement_reflns_used    2312
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1603.8(4)
_computing_cell_refinement       'IPDS1 software (Fa.STOE)'
_computing_data_collection       'IPDS1 software (Fa.STOE)'
_computing_data_reduction        'IPDS1 software (Fa.STOE)'
_computing_molecular_graphics    'ORTEP3 for Windows (L.J.Farrugia 1999)'
_computing_publication_material  'WINGX (L.J.Farrugia 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 2004 ( C.Giacovazzo, 2004)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'IPDS1 diffractometer (Fa.STOE)'
_diffrn_measurement_method       Phi-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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15427
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.8370
_exptl_absorpt_correction_T_min  0.4900
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3681
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                2810
_reflns_number_total             3681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            707893.cff
_cod_data_source_block           ip1_124
_cod_original_sg_symbol_H-M      P(2)1/c
_cod_database_code               8103025