Crystal structures of three (trichloromethyl)(carbamoyl)disulfanes
Goldenberg, Barbara L.; Young Jr, Victor G.; Barany, George; Acta Crystallographica Section E 71 (2015) 1169–1173; doi:10.1107/S2056989015015893

data_2241120
_publ_section_title
;
 Crystal structures of three (trichloromethyl)(carbamoyl)disulfanes
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1169
_journal_page_last               1173
_journal_paper_doi               10.1107/S2056989015015893
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H8 Cl3 N O S2'
_chemical_formula_moiety         'C9 H8 Cl3 N O S2'
_chemical_formula_sum            'C9 H8 Cl3 N O S2'
_chemical_formula_weight         316.63
_chemical_melting_point_gt       357
_chemical_melting_point_lt       359
_chemical_name_systematic
;
(<i>N</i>-Benzylcarbamoyl)(trichloromethyl)disulfane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 103.176(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4247(17)
_cell_length_b                   13.548(2)
_cell_length_c                   8.5675(12)
_cell_measurement_reflns_used    2312
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.92
_cell_measurement_theta_min      2.37
_cell_volume                     1291.2(3)
_computing_cell_refinement
;
SMART (Bruker, 2007)
;
_computing_data_collection
;
SMART (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and <i>Mercury</i>
 (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), PLATON (Spek, 2009),
  <i>ACD/ChemBioDraw</i> (ACD/Labs, 2014)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXTL (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12180
_diffrn_reflns_theta_full        25.076
_diffrn_reflns_theta_max         25.076
_diffrn_reflns_theta_min         1.831
_exptl_absorpt_coefficient_mu    1.009
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.7516
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, (Sheldrick, 2008)
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       rod
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.267
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0157P)^2^+3.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                2056
_reflns_number_total             2284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg2565sup1.cif
_cod_data_source_block           2
_cod_database_code               2241120
_cod_database_fobs_code          2241120
_shelx_estimated_absorpt_t_min   0.752
_shelx_estimated_absorpt_t_max   0.906
_shelx_hkl_checksum              22541
_shelx_res_checksum              53570
_shelxl_version_number           2014/6