[(Pyrrolidin-1-yl)carbothioylsulfanyl]methyl pyrrolidine-1-carbodithioate
Chou, Wei-Lung; Yih, Kuang-Hway; Lee, Gene-Hsiang; Huang, Yen-Hsiang; Wang, Hsiao-Fen; Acta Crystallographica Section E 66 (2010) o3193–; doi:10.1107/S1600536810046027

data_2228247
_publ_section_title
;
 [(Pyrrolidin-1-yl)carbothioylsulfanyl]methyl
 pyrrolidine-1-carbodithioate
;
_journal_coeditor_code           BV2162
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3193
_journal_paper_doi               10.1107/S1600536810046027
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C11 H18 N2 S4'
_chemical_formula_moiety         'C11 H18 N2 S4'
_chemical_formula_sum            'C11 H18 N2 S4'
_chemical_formula_weight         306.51
_chemical_name_systematic
;
[(Pyrrolidin-1-yl)carbothioylsulfanyl]methyl pyrrolidine-1-carbodithioate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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            4
_cell_length_a                   21.9118(18)
_cell_length_b                   4.5705(4)
_cell_length_c                   14.3452(12)
_cell_measurement_reflns_used    2540
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.56
_cell_measurement_theta_min      2.34
_cell_volume                     1436.6(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17016
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.9099
_exptl_absorpt_correction_T_min  0.8560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            light-brown
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.268
_refine_ls_abs_structure_details 'Flack (1983), 1579 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3292
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1007P)^2^+0.6346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1656
_reflns_number_gt                2759
_reflns_number_total             3292
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bv2162.cif
_cod_data_source_block           I
_cod_database_code               2228247
_cod_database_fobs_code          2228247