5-Anilino-4-chloro-3<i>H</i>-1,2-dithiol-3-one
Boukebbous, Khaled; Laifa, El Adoui; De Mallmann, Aimery; Taoufik, Mostafa; IUCrData 1 (2016) x161736–; doi:10.1107/S2414314616017363

data_1544526
_publ_section_title
;
 5-Anilino-4-chloro-3<i>H</i>-1,2-dithiol-3-one
;
_journal_issue                   11
_journal_name_full               IUCrData
_journal_page_first              x161736
_journal_paper_doi               10.1107/S2414314616017363
_journal_volume                  1
_journal_year                    2016
_chemical_formula_moiety         'C9 H6 Cl1 N1 O1 S2'
_chemical_formula_sum            'C9 H6 Cl N O S2'
_chemical_formula_weight         243.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.182(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.9268(6)
_cell_length_b                   20.752(3)
_cell_length_c                   12.3431(19)
_cell_measurement_reflns_used    2296
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.1320
_cell_measurement_theta_min      3.5720
_cell_volume                     992.9(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
CAMERON (Watkin <i>et al.</i>,  1996)
;
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_refinement
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2403
_diffrn_reflns_theta_full        26.452
_diffrn_reflns_theta_max         29.635
_diffrn_reflns_theta_min         3.386
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Rigaku OD, 2015), based on expressions derived by
Clark & Reid (1995)]
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.139
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.79
_refine_diff_density_min         -1.02
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2393
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.0009757
_refine_ls_shift/su_mean         0.0001730
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994; Prince,
1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.173E+04 0.271E+04 0.145E+04 406.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1549
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1549
_reflns_number_gt                1929
_reflns_number_total             2403
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            bt4031sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C9 H6 Cl1 N1 O1 S2'
_cod_database_code               1544526
_cod_database_fobs_code          1544526