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_2241119
_publ_section_title
;
 Crystal structures of three (trichloromethyl)(carbamoyl)disulfanes
;
_journal_coeditor_code           BG2565
_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          'C3 H4 Cl3 N O S2'
_chemical_formula_moiety         'C3 H4 Cl3 N O S2'
_chemical_formula_sum            'C3 H4 Cl3 N O S2'
_chemical_formula_weight         240.54
_chemical_melting_point_gt       352
_chemical_melting_point_lt       353
_chemical_name_systematic
;
(<i>N</i>-Methylcarbamoyl)(trichloromethyl)disulfane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.969(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.1141(16)
_cell_length_b                   13.9234(17)
_cell_length_c                   20.172(3)
_cell_measurement_reflns_used    2920
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.48
_cell_volume                     3638.2(8)
_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      123(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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  0.0299
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21324
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.044
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4168
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0241P)^2^+4.8271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0612
_reflns_number_gt                3556
_reflns_number_total             4168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg2565sup1.cif
_cod_data_source_block           1
_cod_original_cell_volume        3638.3(8)
_cod_database_code               2241119
_cod_database_fobs_code          2241119
_shelx_estimated_absorpt_t_min   0.604
_shelx_estimated_absorpt_t_max   0.861
_shelx_hkl_checksum              68153
_shelx_res_checksum              46204
_shelxl_version_number           2014/6