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_2241121
_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       327
_chemical_melting_point_lt       328
_chemical_name_systematic
;
(<i>N</i>-Methyl-<i>N</i>-phenylcarbamoyl)(trichloromethyl)disulfane
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                81.964(2)
_cell_angle_beta                 81.806(2)
_cell_angle_gamma                68.851(2)
_cell_formula_units_Z            4
_cell_length_a                   8.9231(12)
_cell_length_b                   10.1724(13)
_cell_length_c                   15.364(2)
_cell_measurement_reflns_used    2932
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.46
_cell_volume                     1281.5(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      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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  0.0342
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15282
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         1.345
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6761
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+0.6770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                4557
_reflns_number_total             5790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bg2565sup1.cif
_cod_data_source_block           3
_cod_database_code               2241121
_cod_database_fobs_code          2241121
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.914
_shelx_hkl_checksum              64373
_shelx_res_checksum              50010
_shelxl_version_number           2014/6