Crystal structure of bis(<i>N</i>-methyl-<i>N</i>-phenylamino)trisulfane
Barany, George; Henley, Matthew J.; Polski, Lauren A.; Schroll, Alayne L.; Young, Jr, Victor G.; Acta Crystallographica Section E 71 (2015) 836–839; doi:10.1107/S2056989015011342

data_2240864
_publ_section_title
;
 Crystal structure of bis(<i>N</i>-methyl-<i>N</i>-phenylamino)trisulfane
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              836
_journal_page_last               839
_journal_paper_doi               10.1107/S2056989015011342
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C14 H16 N2 S3'
_chemical_formula_moiety         'C14 H16 N2 S3'
_chemical_formula_sum            'C14 H16 N2 S3'
_chemical_formula_weight         308.47
_chemical_melting_point          353
_chemical_name_common            03251a
_chemical_name_systematic
;
Bis(<i>N</i>-methyl-<i>N</i>-phenylamino)trisulfane
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   19.284(3)
_cell_length_b                   56.440(8)
_cell_length_c                   11.1695(15)
_cell_measurement_reflns_used    1945
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.38
_cell_volume                     12157(3)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0823
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       67
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15884
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.9812
_exptl_absorpt_correction_T_min  0.8904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             5184
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.312
_refine_ls_abs_structure_details
;
2194 Friedel pairs (Flack, 1983)
;
_refine_ls_abs_structure_Flack   0.08(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+36.8709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1062
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                3097
_reflns_number_total             4978
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su5144sup1.cif
_cod_data_source_block           I
_cod_database_code               2240864
_cod_database_fobs_code          2240864